Dheyab2020 PDF

Chinese Journal of Physics 64 (2020) 305–325
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Chinese Journal of Physics

journal homepage: www.elsevier.com/locate/cjph
Synthesis and coating methods of biocompatible iron oxide/gold

T
nanoparticle and nanocomposite for biomedical applications
⁎ ⁎
Mohammed Ali Dheyaba,b, , Azlan Abdul Aziza,b, , Mahmood S Jameela,b,
Osama Abu Noqtaa,b, Baharak Mehrdela,b
a
Nano-Biotechnology Research and Innovation (NanoBRI), Institute for Research in MolecularMedicine (INFORMM), Universiti Sains Malaysia,
11800 Pulau Pinang, Malaysia
b
Nano-Optoelectronics Research and Technology Lab (NORLab), School of Physics, Universiti Sains Malaysia, 11800 Pulau Pinang, Malaysia
A R T IC LE I N F O ABS TRA CT
Keywords: This detailed review presents an overview of current research on the synthesis, surface mod-
Iron oxide (Fe3O4) ification, and applications of Iron oxide (Fe3O4) nanoparticles and iron oxide/gold (Fe3O4/Au)
Core/shell nanocomposite nanocomposites. The different synthesis techniques of Fe3O4 with various basic organic and in-
Surface modification organic modifications are presented. The applicability and role of inorganic and organic coating
Au coated Fe3O4
on iron oxide/gold core/shell schemes were explored. The trade-off between choices for surface
Biomedical applications
functionalization related to specific applications such as imaging contrast agent, drug delivery
carrier and therapeutic device using iron oxide/gold core/shell was also elaborated. The versa-
tility of combining iron oxide/ and gold as nanocomposite as the choice for biomedical appli-
cation is demonstrated in MRI, CT scan, drug delivery, biosensors, and hyperthermia application.
1. Introduction
Composite nanoparticles that comprise of distinct functional components play an important role in biomedical applications due to
their exceptional physicochemical features. Iron oxide/gold (Fe3O4/Au) nanocomposite is one of the most important nanoparticles,
utilized for diverse biomedical applications that include photothermal therapy [1], targeted drug delivery [2], (CT/MRI) dual-
modality [3], biosensing [4], catalysis [5], and immunoassays [6]. The use of Fe3O4 nanoparticles in these applications is based on
their relatively low toxicity, slow oxidation, high saturation magnetization, and higher magnetic susceptibility compared to ma-
ghemite (γ-Fe2O3). These properties of nanoparticles can be altered by reactive groups and various charges on the surface of particles,
thus improving compatibility and stability [7]. Therefore, the effectiveness and variability in the applications of these Fe3O4/Au
nanocomposites are significantly dependent on their composition, stability, dispersity and the nanostructure under different con-
ditions.
Fe3O4 nanoparticles with a grain size of smaller than 20 nm display superparamagnetic behavior (SPIONs) at high temperatures.
Furthermore, these particles exhibit no coercivity and remanence, while the agglomeration effect of these particles is insignificant at
room temperature [8]. However, the uncoated Fe3O4 nanoparticles have several drawbacks when used for biomedical applications,
which include its formation of harmful free radicals [9], ineffective surface binding of the ligand that results in failure of drug
delivery [10] and instability under physiological conditions [11]. To resolve these challenges, Fe3O4 nanoparticles need to be coated
⁎
Corresponding authors at: Nano-Biotechnology Research and Innovation (NanoBRI), Institute for Research in MolecularMedicine (INFORMM),
Universiti Sains Malaysia, 11800 Pulau Pinang, Malaysia.
E-mail addresses: mohammed@student.usm.my (M.A. Dheyab), lan@usm.my (A.A. Aziz).
https://doi.org/10.1016/j.cjph.2019.11.014
Received 5 April 2019; Received in revised form 15 October 2019; Accepted 20 November 2019
Available online 27 November 2019
0577-9073/ © 2019 The Physical Society of the Republic of China (Taiwan). Published by Elsevier B.V. All rights reserved.
M.A. Dheyab, et al. Chinese Journal of Physics 64 (2020) 305–325
with suitable materials that can enable biocompatibility [12].

The incorporation of Au nanoparticles into Fe3O4 nanoparticles is one of the most exciting potential modifications to be used for
biomedical applications due to its simple synthesis, enables good biocompatibility, and provides many possible options of bio-
conjugation. In addition, the surface plasmon resonance (SPR) optical property of the Au nanoparticles ensures high optical ab-
sorption in the UV and NIR region [13]. The inclusion of Au nanolayers creates a high intensity and distinct optical spectral response,
where the localized surface plasmon frequency is influenced by the dielectric and morphological properties of a core and the local
surrounding medium [14,15]. To better understand the synthesis of Fe3O4 nanoparticles, different wet chemical methods will be
deliberated. Given the instability of Fe3O4 for biomedical applications, a layer (Au layer) applied around the Fe3O4 nanoparticles is
the preferred strategy to improve Fe3O4 stability and biocompatibility. The modification of Fe3O4 nanoparticles by adding an Au
layer to form Fe3O4/Au nanocomposites will now be further elaborated.
Firstly, the different synthesis methods of Fe3O4 nanoparticles were discussed, which include co-precipitation, electrochemical,
hydrothermal, microemulsions and reverse micelles, sol-gel, solvothermal, sonication and thermal decomposition. The second section
covers the synthesis of bi-layer and multilayers of Fe3O4/Au core/shell nanocomposites. The third section discusses the surface
modification of Fe3O4 nanoparticles with organic and inorganic compounds to form Fe3O4/Au nanocomposites, which are suitable for
biomedical applications such MRI, CT scan, drug delivery, biosensors, and hyperthermia. Therefore, this review analyzes the fun-
damental requirements for effectively synthesizing Fe3O4/Au nanocomposite materials, appropriate for biomedical applications. This
study is important since published reviews, thus far, have only highlighted the chemical aspects, such as synthesis, characterization
and biomedical applications, with the aim of developing successful contrast agents for molecular imaging. Those studies also gen-
erally describe the physicochemical properties of nanoparticles without focusing specifically on iron oxide particles. For this reason,
the main objective of this review is to elucidate the synthesis and characterization of all physicochemical properties and surface
modifications of iron oxide nanoparticles with emphasis on their biomedical applications, particularly in the field of molecular
imaging, such as MRI and CT scan in addition to drug delivery, biosensors and hyperthermia.
2. Wet chemical methods for the synthesis of magnetite nanoparticles
There are several widely reported chemical methods for the synthesis of Fe3O4 nanoparticles for biomedical applications namely,
co-precipitation, electrochemical, hydrothermal, microemulsions and reverse micelles, sol-gel, solvothermal, sonication and thermal
decomposition. In general, all agree that the synthesis of Fe3O4 nanoparticles is a complicated process due to their colloidal nature.
The advantages, disadvantages and features of the obtained Fe3O4 products from each method are summarized in Table 1. The main
challenges of these methods consist of determining the experimental conditions for synthesizing monodisperse of Fe3O4 grains with
the desired size. These chemicals methods have been successfully employed to synthesize nanoparticles with narrow size distribution
and homogeneous composition. Fig. 1 shows extensive synthetic methods of Fe3O4 nanoparticles along with its surface modifications.
2.1. Co-precipitation method
Co-precipitation method is one of the most important and common chemical wet methods for the preparation of Fe3O4 in addition
to controlling the size and shape of the aqueous solution [16]. It is also the simplest chemical reaction to produce superparamagnetic
iron oxide nanoparticles, SPIONs [17]. Strong base solution such as NaOH, NH4OH and KOH are added to the solution to facilitate the
chemical process at room temperature [18,19], while the weak base such as Na2CO3 is used for a very slow reaction [20]. The
preparation of Fe3O4 via co-precipitation method involves the reaction between ferric and ferrous with at ratio 2:1 or 1:1 with
vigorous stirring in an aqueous media [21,22]. The type of precipitating agent plays a significant role in determining the physico-
chemical and magnetic properties of Fe3O4 nanoparticles [23]. When strong alkaline media such as LiOH, KOH, and NaOH are used
as hydrolyzing agents, an impurity such as Goethite (αFeO(OH)) is observed but virtually absent when ammonia (NH3) is utilized
[24]. The impurity effects and contributes to a decrease in the magnetic moment the particles [25]. Several organic materials served
as a peptizing agent in Fe3O4 nanoparticle syntheses such as a Citric acid (C6H8O7), nitric acid (HNO3), perchloric acid (HCI4), and
tetramethylammonium hydroxidean (C4H13NO) to prevent agglomeration of Fe3O4 nanoparticles by electrostatic repulsion [26].
Eventually, these substances are incompatible with biomedical application because they possess unacceptable percentage of toxicity.
Previous studies have shown that the size of Fe3O4 particles can be controlled by adjusting the reaction conditions such as reaction
time, the ratio of concentration Fe2+/Fe3+, pH, temperature, ionic strength in the medium and stirring speed [26–28]. The saturation
magnetization is directly proportional to the size of the Fe3O4 where the magnetism will decrease when the particle size is small [29].
The main drawbacks of the co-precipitation method are the agglomeration and polydisperse of Fe3O4 nanoparticles. However, re-
cently many researchers have revealed that the presence of polymers in chemical reactions can assist a successful synthesis of highly
monodisperse and non-agglomeration Fe3O4 particles via steric repulsion [30,31]. In other words, the polymer works to separate the
nucleation and growth process as a capping agent and prevents growth after the process of nucleation. The co-precipitation used
NaOH can be easily implemented and requires less time and has the highest yield. Nonetheless, the same cannot be said about when
NH3.H2O is used. Results show that smaller size and low output yield was obtained, and longer synthesis time was required [32].
During the preparation process, it is preferable to have an N2 gas to protect the product from oxidation a with desired temperature. At
the end of the process, according to previous studies, a quick visual indicator for good Fe3O4 is black [33].
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M.A. Dheyab, et al.
Table 1
Comparison between synthesis methods in preparation Fe3O4.
Method Features of the obtained Fe3O4 Reaction condition Advantage Disadvantage Yield Ref.
products
Co-precipitation Magnetization value: 20-80 emu/g Temperature: 20-90°C Facile, simple, easy, low cost and controllable size. Agglomeration and difficult to avoid nucleation High [128]
Size distribution: Broad Duration: Minutes during the reaction
Shape control: Not good
Electrochemical Magnetization value: 35.5 emu/g Temperature: Room Facile, high purity and particle size can be Complex procedure Medium [35]
Size distribution: Medium temp controlled
Shape control: Medium Duration: Hours-days
Hydrothermal Magnetization value: 20-80 emu/g Temperature: 150- Facile, crystalline, highly pure and The crystal growth cannot be controlled High [129]
Size distribution: Very narrow / 220°C environmentally friendly
Narrow–broad Duration: Hours-days
Shape control: Very good
Microemulsions Magnetization value: up to 113 Temperature: 20-50°C Uniform and thermodynamically stable Complex and heterogeneous Low [62]
emu/g Duration: Hours nanoparticles
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Size distribution: Narrow
Shape control: Good
Sol-gel Magnetization value: 10-40 emu/g Temperature: 25-200°C Desired shape and hybrid nanoparticles The product contains a sol-gel mixture component Medium [130]
Size distribution: Narrow Duration: Hours
Shape control: Good
Solvothermal Magnetization value: up to 108 Temperature: 150- High Purity, good crystallinity Relatively slow kinetic and sensitive to the High [85, 130]
emu/g 220°C concentrations of alkalinity and water
Size distribution: Narrow-broad Duration: Hours-days
Shape control: Good
Sonication Magnetization value: 63 emu/g Temperature: 20-50°C Facile, rapid and environmental friendly Amorphous nanoparticles Medium [131]
Size distribution: Narrow Duration: Minutes
Shape control: Bad
Thermal decomposition Magnetization value: up to 91 emu/ Temperature: 100- Monodispersed, inexpensive and high quality of Complicated and requiring high temperatures High [132]
g 320°C Fe3O4 nanoparticles
Size distribution: Very narrow Duration: Hours-days
Shape control: Very good
Fig. 1. Represented various methods of producing Fe3O4 and its surface modifications with organic and inorganic materials.
2.2. Electrochemical method
The electrochemical process of producing superparamagnetic iron oxide nanoparticles (SPIONs) is based on oxidation and re-
duction reaction of iron which base electrolyte's in an electrolyte. The electrochemical method has also been utilized to generate
various Fe3O4 nanoparticles phases such as magnetite (Fe3O4) and maghemite (Fe2O3) nanoparticles [34]. This phenomenon can be
explained by crossing an electric current through two electrodes (anode and cathode). More so, the positively charged electrode
(anode) can be oxidized to metal ion species inside the electrolyte and the metal ion is later reduced to metal by the negatively
charged electrode (cathode) with the assistance of stabilizers. The Fe3O4 nanoparticles is deposited on the electrode normally in the
form of a coating or a thin film. The synthesis of Fe3O4 nanoparticles via this method does not require high temperature and the
electrolyte's temperature must be less than the boiling point. At room temperature, this method has a disadvantage, often produces
poorly ordered particles that cause an explicit structural characterization hard [35].
2.3. Hydrothermal method
Hydrothermal method is one of the most common wet chemical ways for the synthesis of inorganic nanocrystals, especially for
metal and metal oxides [36,37]. The formation of Fe3O4 nanoparticles involves two steps; Firstly, the hydrolysis reaction and then the
dehydration process as demonstrated in Eqs. (1) and (2) [38].
Hydrolysis: Mn+ +nH2O → M(OH)n + n H+ (1)
Dehydration: M(OH)n → MOn/2 + n/2 H2O (2)
This method often utilizes relatively high temperature and pressure to influence the formation of nanocrystals. It includes the
heating of a water solution of iron salt at a temperature and pressure of 374 °C and 22.1 MPa, respectively. The hydrothermal process
has a varied advantage such as facile control, environmentally friendly process, good crystallization and morphology of products. In
addition, under this high pressure, some metastable and condensed phases can be produced. With regard to magnetic nanoparticles,
nanosheets, nanorods, nanowires, nanoplates, nanospheres, nanorings, nanocubes, etc. have been successfully prepared via the
hydrothermal synthetic process [39–48]. Fe3O4 nanoparticles with an average of 50 nm have been prepared by utilizing Na2S2O3 as
the control agent via the hydrothermal method.
The synthesizing of the Fe3O4 nanoparticles phase depends on the ratio of Na2SO3 to FeSO4 [49]. Fe3O4 nanoparticles with size
27 nm in the presence of a suitable surfactant via hydrothermal process have been prepared [50]. Previous studies demonstrated
microwave hydrothermal with a temperature range of 90 to 200 °C have demonstrated a spherical Fe3O4 nanoparticles with size
ranged between 150 and 200 nm by using the FeCl3 and FeSO4.7H2O as precursors and NaOH as hydrolysis reactant. It was found the
formation of Fe3O4 nanoparticles controlled by a critical parameter (Fe/NaOH). Chen et al. reported that Fe3O4 nano-powders
prepared via a hydrothermal process by employ Fe2+ precursor (FeCl2•4H2O). They used the FeCl2 to react with the mixing of N2H4
and NaOH thus the iron salts Fe2+ and Fe3+ had partially oxidized by N2H4 [51].
The hydrothermal method also used the Polyvinylpyrrolidone (PVP) as the surfactant where the shape of Fe3O4 nanoparticles can
be controlled by mixing FeSO4.7H2O, NaOH, FeCl3 with benzene and PVP. By varying PVP amount and experimental conditions,
Fe3O4 nanoparticles with different morphologies can be obtained, like nanowires, nanorods, nanoparticles and mixtures [52].
However, the disadvantage of this method is the slow reaction kinetics at any proposed temperature. Therefore, microwaves assisted
hydrothermal process was proposed [53]. The microwave heating process provides increased interaction kinetics and improved
crystallization of the sample. By combining of two process hydrothermal effects and microwave irradiation, the morphology of
synthesized SPIONs can be adjusted or controlled. SPIONs with cubical shaped or rhombohedral, hexagonal were reported [54]. In
308
Fig. 2. Shows the formation of nanoparticles via w/o microemulsions [70].
this study, the hydrothermal method recorded many advantages features such as high yield, controllable size, excellent particle
crystallinity and good morphology [38].
2.4. Microemulsions and reverse micelles method
A stable or thermodynamically stable system consists of two liquids immiscible such as oil and water in addition to the presence of
surfactant aggregate [55]. There are three types of microemulsions; firstly, direct oil in water microemulsion (o/w), secondly, re-
versed water in oil (w/o), and thirdly, bicontinuous. This classification depends on the hydrophilic-lipophilic balanced value and the
ratio of water to oil (w/o) [56]. Nanoparticles formation under the microemulsion method undergoes four phases. I), mixing of
microemulsion components II), exchange of substances through the nano-droplets, III) reaction nucleation and IV), reaction out-
growth [57]. Particle stability via this method is influenced by the amount and type of surfactant, and the pH of the dispersing
medium [58].
As demonstrated in Fig. 2, when two nanoparticles collided together, the reactants would be exchanged for the formation of
nanoparticles by the Brownian movement [59]. A water droplet covered with a suitable surfactant is called a nanoreactor. More
importantly, the surfactant prevents water droplets from forming excess aggregation [60]. Recently, a study has demonstrated that
the microemulsion process can synthesize monodisperse SPIONs by varying the concentration of precursor and size of the droplet
radius, as shown in Fig. 3H [61]. SPIONs can be prepared through two methods firstly, water in oil (w/o) and the second oil in water
(o/w) via microemulsions process [62–66]. In another method, the conventional method of synthesis SPIONs via microemulsion need
to adding reducing agent such as ammonia to reactants [67]. The size distribution and shape can be controlled by manipulation in the
amount of surfactant, water and oil via microemulsion process [68,69], while using different temperatures during the reaction
produced Fe3O4 nanoparticles with a diameter in the range of 3 to 12 nm [70]. Jia et al. reported a new procedure by adding basic
solution NaOH as reducing agent to produce Fe3O4 surrounded by chitosan. The size of this component ranged from 10 to 80 nm [71].
Similar to the problem observed in the co-precipitation method, the main disadvantage is the agglomeration and inability to
monodispersed the particles and to precisely control the size. Furthermore, a large amount of dissolvent is necessary to synthesize a
ratable amount of nano-materials and to reverse the effects of residual surfactants on the property of the particles [72]. In order to
overcome those limitations, oleic acid can be added to the reactants as stabilizing agents [73]. The main advantage of this method is
that it is environmentally friendly and economical [74]. More importantly, the SPIONs synthesized via this method depends on
droplet size, surfactant and the concentration of reactant [75].
2.5. Sol-gel method
In chemical wet approaches, sol-gel is one of the techniques for producing Fe3O4 nanoparticles with unique properties [76], which
involves hydroxylation and condensation of precursors and thus turn into an inorganic solid [77]. Fe3O4, prepared via sol-gel, is very
high purity and homogeneous [78].The morphology and structure can be adjusted by adjusting the parameter such as the con-
centration of the salt precursors, pH, agitation and temperature [79]. However, the change in pH also affects the magnetic properties
309
Fig. 3. TEM of Fe3O4 synthesized by (A) Co-precipitation [132] (B) Electrochemical [34] (C) Hydrothermal [133] (D) Microemulsion [134] (E) Sol-
gel [135] (F) Solvothermal [44] (G) Sonication [136] (H) Thermal decomposition [137].
of the resulting materials [76]. There are four steps in synthesizing Fe3O4 nanoparticles using this method; (a) hydrolysis and poly-
condensation of iron precursor in a solvent to form a colloidal suspension of the particles (sol), (b) gelation of the sol to form a gel, (c)
the aging and (d) drying of the particles. Nevertheless, similar to the co-precipitation process, the sol-gel is challenged to produce
monodisperse particles and prevent the agglomeration. To overcome both limitations several improvements have been reported to
the synthesis of monodisperse and non-agglomerated via sol-gel process. Dong and Zhu. have been recorded that polyethylene glycol
(PEG) can be used as a capping agent to mitigate the agglomeration and give the uniform size of Fe3O4 nanoparticles [80]. The sol-gel
method has been prepared to synthesis nanocomposite materials by using aqueous way [81]. The method used in this study has
several merits. Firstly, its ability to monitor the fine structure identity of the reaction outputs. Secondly, its ability to get a pure
amorphous stage, solo-dispersity, and well monitoring of the particle diameter. Thirdly, it's possible to get items with a prearranged
shell regarding empirical situations.
2.6. Solvothermal method
A solvothermal method involves presenting the organic solvent like ethanol, methanol or polyol at an extremely high temperature
and pressure [82]. Recently, many authors demonstrated that SPIONs had been synthesized by a solvent such as hydrazine (N2H4)
and ethylenediamine (C2H8N2) [45,83,84]. The morphology and good uniformity in this method result from the reaction between the
iron precursor and surfactant [85]. J. Liang et al have been demonstrated that the size of Fe3O4 nanoparticles can be controlled by
changing in the ratio of surfactant, the concentration of NaOH, and precipitator [86]. In the solvothermal technique, the dispersity of
iron salts, the temperature of reaction and the aging time are crucial parameters in determining the size distribution and controlling
the nucleation and growth processes [87,88]. Various surfactants such as sodium dodecylbenzene sulfonic [86], oleic acid [89] and
polyacrylic acid [86] have been utilized as capping agents to preparation Fe3O4 nanoparticles with high monodispersity. The Fe3O4
nanoparticles that was prepared by this method are hydrophilic which can be dispersed in an aqueous solution or polar solvents [90].
The advantages of this method include no requirement for any surfactant or reducing agents except liquid polyols and control
experimental conditions [91].
2.7. Sonication method
Sonication method (sonochemical or sonolysis) is a facile way to synthesize SPIONs and other nanostructure by decomposition
(sonolysis) of an inorganic iron precursor using very high temperature and pressure generated by ultrasonic irradiation, up to 5000 K
and 2000 atm, respectively [92]. The ultrasonic irradiation produces high temperature leads to generates magnetic nanoparticles by
decomposition iron salts [93]. Hydrophilic and monodisperse properties of SPIONs have been improved via sonication method
[94,95]. Recently, many authors reported the presence of an appropriate stabilizer to contribute to synthesis SPIONs with high
dispersed via ultrasonic irradiation [96,97]. The sonication method often produces an amorphous shape because of the high tem-
perature and pressure resulting from this process [97,98]. More importantly, during the formation process of SPIONs, the acoustic
cavitation process inhibits crystallization. More so, the crystalline properties of the SPIONs can be controlled by heat treatment [99].
310
The synthesizing of SPIONs with crystalline properties at low ultrasonic temperature also has been recorded [100–102]. Several
parameters are crucial for the synthesize Fe3O4 nanoparticles by this method such as temperature, time, sonication frequency to
control the size distributions and morphology [99].
2.8. Thermal decomposition method
The thermal decomposition technique is a well famous process for synthesis monodisperse and highly crystalline of SPIONs
[103–105]. It involves the decomposition of the precursors of iron by very high temperatures [106,107]. In addition, the crystallinity
and magnetic properties of SPIONs can be obtained by increasing the mixture reaction up to 300 °C [108]. The iron precursors such as
acetates [109], oxalates [109], oleates [109], carbonyl [110] and ferrocene [110] can be used in this process while benzyl ether
utilized as boiling solvent [111]. During the thermal decomposition process, the nanoparticles undergoes two important routes for
control nucleation and growth mechanization. Firstly, involve direct injection of organometallic compounds in hot surfactant solution
that results in the immediate formation of nuclei. Secondly, involves control heating of these compounds in surfactant solution for
nuclei formation [112]. Park et al., Roca et al. and Baaziz et al. have reported that the precursor concentrations and the ratio of Fe/
oleic acid are as critical parameters in controlling nanoparticles size [113–115]. A high-temperature reaction of Fe2O3 acet-
ylacetonate with 1,2-hexadecanediol in existence oleylamine and oleic acid is needed to acquire monodisperse magnetite nano-
particles. In presence of a bipolar surfactant, the hydrophobic nanoparticles can be converted into hydrophilic and the diameter of
particles also tuned from 4 to 20 nm [116]. N.R. Jana et al and M. Mohapatra et al have been proposed the use of non-toxic FeCl3 and
FeCl2 salts as a precursor [117,118].
Recently, thermal decomposition method producing a water-dispersible magnetic nanoparticles in acidic have been synthesized
using FeCl3 [119] and Fe(acac)3 [120–123]. The diameters nanoparticles of 4,12 and 60 nm can be controlled according to the time of
reflux (condensation of vapors and the return of this condensate to the system) [119]. Interestingly, the shape of nanoparticles from
spherical to cubic has been changed by increasing the time of reflux. The synthesis of Fe3O4 via thermal decomposition method
requires further investigation on the mechanism of chemical conversions because the reaction mixtures produced contain multi-
component reactions e.g. different kind of components was produced during the oxidative of Fe (II) including iron Fe3O4, γ- Fe2O3,
FeO, (α-Fe), α-Fe2O3, siderite (FeCO3) and iron carbide(Fe3C) [124]. The advantages of thermal decomposition are, inexpensive iron-
organic precursor and very short reaction time. Thermal decomposition process also has some disadvantages such as complicated
procedures [82], emission of toxic gases such CO [125], uses toxic and expensive reagents (not environmental friendly) [126],
required high reaction temperature [82], uses the multiple reagents [82] and the inability to get required nanoparticle size [127].
Future development of this method should strive towards the synthesis of water-soluble magnetic nanoparticles directly that uses less
reagents.
3. Synthesis of Fe3O4/Au Core/shell nanocomposite
Surface modification of Fe3O4 nanoparticles with a suitable shell is a necessary action for the various application of Fe3O4 for
three reasons: (i) being nanometer sizes, the ratio of the surface to volume makes them highly active which require surface mod-
ification to minimize the surface energy for keeping the appropriate chemical stability, (ii) the advantages of Fe3O4 become available
only when it is well dispersed in the solution; therefore, the modification is effective to prevent the agglomeration and (iii) most
importantly, Fe3O4 with an appropriate ligand is necessary for most applications including manipulation of cells and proteins.
Noteworthy in this article, we reviewed two effective approaches to synthesis Fe3O4/Au nanoparticles: the first approach is bi-layer
which structure consists of two layers: Fe3O4 in the core and Au as a shell. The second is a multilayer composite structure (Fig. 4). The
multilayer composite structure consisting of at least three layers including the core, glue material such as metal or organic material
and Au shell. Fe3O4/Au nanoparticles can be prepared by two different approaches. The first approach employs to produce a bilayer
structure (Schema I) and the multilayer approach employ to produce multilayer composite nanostructures (Schema II).
3.1. Synthesis of a Fe3O4 bi-layer structure
Recent studies have deliberated that the formation of an Au shell can be obtained in two ways. Firstly, a method is a one-pot
synthesis where the Au ions grow to form a shell on the Fe3O4 surface. Secondly, the Au nanoparticles are grown outside and then
added to the Fe3O4 suspension and form the Au shell on the surface. The first way is fast, simple and one pot of shell-formation. The
Au precursor is reduced on the Fe3O4 surface by using the reducing agents that leads to formation of Au shell on the surface or
separately in the system, and shell formation in this way is a non-uniform and non-continuous shell or seeds. While the second way is
complex but effective in forming a uniform and continuous shell. The accuracy of the forming shell depends on the ratio and of Au
precursor concentration in the solution to reducing agents. Judging from the recent trend in publication, it shows that Fe3O4/Au is
most preferably synthesized using the second method [133–138]. For instance, Fe3O4 nanoparticles with size 9-20 nm were syn-
thesized by co-precipitation FeCl3 and FeCl2 salts in diluted NH3 solution. The extracted Fe3O4 nanoparticles were then added to
boiling HAuCl4. In addition, L-Homocysteine was later added to the solution to form Fe3O4/Au/homocysteine nanoparticles (shown
in Table 2) [135,139]. These nanoparticles are water-soluble, which is a requirement for biomedical applications. The carboxylate
and amine groups formed on the surface of particles may allow sequent transformations as carboxylated Fe3O4/Au nanoparticles
[134] and for an Au nanoparticles ligand sphere [140]. Based on transmission electron microscopy (TEM) data was obtained, Fe3O4
nanoparticle geometry is an almost spherical shape with sizes around 12.3 nm [139] and 22 nm [135]. Fe3O4 nanoparticles coated
311
Fig. 4. Schematic representation of two approaches for synthesis Au coated Fe3O4.
with Au can also be employed NaBH4 to the reduction of HAuCl4 in the presence of sonicator.
The sonication technique leads to prevents the agglomeration and improved the nanoparticles monodispersity due to ionic in-
teractions. According to TEM image (Fig. 5A), the average size of the resulting mixed metal core/shell nanoparticles is 12.573 nm
[141]. Hydroxylamine hydrochloride (HONH2.HCl) also can be utilized as a reducing agent. Hydroxylamine hydrochloride and
sodium citrate employed in synthesizing Fe3O4 coated with Au. This technique requires a longer time compared with the other
methods [139,141] and takes approximately 5 hours. This process produces nanoparticles with a size of 20 nm and spherical in shape
[142]. The first step includes adding sodium citrate to Fe3O4 and stirred this solution before adding HAuCl4 and NH2OH.HCl for
30 min. The next step includes modifying the Fe3O4/Au with 3′(alkanethiol) oligonucleotides, which then produced nanoparticles
with the average size of 100 nm to be used in DNA detection [143]. The Fe3O4 surface can also get modified with sodium citrate to
attract Au ions. Using this approach the average diameter of Fe3O4/Au core/shell obtained ranged from 15 to 40 nm. In the synthesis,
Fe3O4 nanoparticles were first prepared via the co-precipitation process, then sodium citrate added to the solution before the rinsing
the precipitate and left stirred continuously [136, 144]. Similar to the previous approach, the HAuCl4 solution was heated to boil, and
then Fe3O4 nanoparticles covered with sodium citrate were added to the mixture [144]. Another interesting modification of this
approach involves the sonication of Citrate and Fe3O4 nanoparticles and heating them till boiling before adding HAuCl4; this
synthesis takes up 15 minutes after adding HAuCl4 [144].
Alternatively, the citrate can be added to the Fe3O4 solution after rinsing the precipitate. In this condition, the exchange of OH−
with citrate anions took up overnight [137] compare with other methods [136,144,145]. After the extended soaking time, HAuCl4
was then added to the mixture with the assistance of hydroxylamine as a reducing agent. The methods that were described in this part
are rapid and convenient because all the reactions take place in an aqueous solution. Fe3O4/Au synthesis in organic media with a
diameter of particles 6.7 ± 0.7 [146] and 10 nm [138] was prepared by thermal decomposition method. Oleylamine and oleic acid
served as capping agents to formation Fe3O4 nanoparticles, whereas the presence of amine groups on the surface of nanoparticles was
employed as a template to facilitate the attaching of Au3+ ions through the thermal decomposition process. Xu et al. reported the
oleylamine had been used to reduction HAuCl4 in the presence of Fe3O4 to formed the Au shell [138]. These nanoparticles non-
dispersed in the polar solvent. To make the mixture water-soluble, it was dissolved in an aqueous solution of sodium citrate and
cetyltrimethylammonium bromide (CTAB) under sonication. The core diameter of 10 nm with various diameters of a shell (1, 1.5, 2,
2.5 and 3 nm) was obtained by using ascorbic acid to reduce HAuCl4 [138]. This method requires temperature control and takes a
long time compared to the reduction method by employing hydroxylamine or sodium citrate. The main advantage of this method is
that the thickness of the Au shell can be controlled.
Another synthesis approach in achieving Fe3O4/Au core/shell is by reverse micelle method. In this method, Fe3O4/Au nano-
particles were prepared under argon by using CTAB as a surfactant, 1-butanol as co-surfactant and octane as an oil phase [147]. The
Fe cores could be prepared from FeSO4 by using NaBH4 as a reducing agent. To form Au shell on Fe core, HAuCl4 was prepared as
micelle solution, then added to the solution of NaBH4 and FeSO4 and left stirring overnight at room temperature. This process showed
that the diameter of nanoparticles was 18 ± 4. The surplus of NaBH4 appears as a negative charge on the Au surface which in turn
prevents the seed from agglomeration and also helps to attract them to the Fe3O4 surface through electrostatic interaction. Maleki
et al. described another technique for synthesis Fe3O4/Au nanoparticles through pre-adsorbed Au seeds. This technique includes the
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M.A. Dheyab, et al.
Table 2
Comparison between various synthesis approach.
Core/shell Approach Synthesis methods Size Applications Refs
Core Shell Core nm particle
Fe3O4/Au I Co-precipitation Reduction by citrate 20 22 (2 nm gold shell) T2 in MRI [135]

Fe3O4/Au I Thermal decomposition Reduction byoleylamine 6.7 ± 0.7 9.2 ± 1.3 (1 nm gold shell) Unspecified [146]
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Fe3O4/Au I Reversed micelle technique Reduction by NaBH4 6 4–22 (3nm gold shell) DNA sensors [134]
Fe3O4/PZS/Au II sonication Reduction by NaBH4 8.2 ± 1.1(Fe3O4) 228.5 ± 15 (Fe3O4 /PZS) 253 ± 20 (3nm Au NPs) Photothermal and MRI [149]
Fe3O4/PB/Au II Co-precipitation Reduction by citrate Less than 10 80 (1-3nm Au NPs) immunosensors [149]
Fe3O4/PANI/Au II Solvothermal Reduction by NaBH4 170 3 (Au NPs) Unspecified [152]
Fe3O4/PEI/Au II From KNO3 and FeSO4 Reduction by NH2OH.HCl 20 30 ± 5 (4 ± 1 nm Au NPs) Bioseparation [150]
Fig. 5. TEM image of (A) Fe3O4/Au nanoparticles bi-layer [140], (B) Fe3O4/PZS/Au [148], (C) Fe3O4/PB/Au [153], (D) Fe3O4/PANI/Au [151] and
(E) Fe3O4/PEI/Au [149] multilayer.
attaching of Au seeds to the surface of Fe3O4. Fe3O4 nanoparticles act as nucleation sites to form the Au shell and the reducing agent
[148].
3.2. Synthesis Fe3O4/glue/Au multilayer
The approach of multilayer nanocomposites is different from the methods described earlier. Multilayer nanocomposites structure
possesses a “glue layer” between the Fe3O4 core and Au shell. Various materials can be used as glue, such as polymers [149–152],
silica [153] and others [154]. The main role of the glue layer is to hold the Fe3O4 nanoparticles in place and prevents them from
aggregating. Besides, the glue layer must be stable and biocompatible. As such, the synthesizing scheme of glue layer is very im-
portant to achieve multifunctional nanosystems. Polyphosphazene (PZS) is one of the suitable glue layers because it possesses
phenolic hydroxyl groups and has a lot of atoms such N, P, and S. The Fe3O4 nanoparticles were prepared from the precursor of iron
Fe(acac)3 under polyol medium triethylene-glycol and high temperature. A mixture of Fe3O4, triethylamine and hexachloro-cyclo-
triphosphazene in the existence of tetrahydrofuran maintained through ultrasonic irradiation. It is followed by adding the PZS and
then keep under irradiation for 6h. Then Fe3O4/PZS nanoparticles were collected and add them to HAuCl4. This mixture stays for
30 min under ultra-sonication, sodium citrate and NaBH4 were added. The geometry images obtained by TEM showed the diameters
of Fe3O4 nanoparticles, core/shell nanoparticles Fe3O4/PZS and Fe3O4/PZS/Au at 8.2 ± 1.1 nm, 228.5 ± 15 nm and 253 ± 20 nm
respectively (Fig. 5B)[149].
Prussian Blue (PB) is also another material that can be used as a glue layer. In biosensing applications, PB could help to accelerate
the transfer of electrons between the electrodes and enzymes [155]. Work by Dobson and Lee et al. suggested that Fe3O4/PB is
suitable for biomedical applications [156,157]. The synthesis of Fe3O4/PB/Au nanoparticles include two steps, firstly Fe3O4 was
obtained by co-precipitation method then Fecl3 and K3[Fe(CN)6] in the presence of HCl have been used to produce Fe3O4/PB. Next,
Fe3O4 was modified with Bovine serum albumin to obtain amine groups on the surface of the nanoparticle. Subsequently, Fe3O4/PB
attracted Au seeds to formation Au shell by citrate reduction. Based on TEM images, the diameter of Fe3O4 and Fe3O4/PB/Au were
10 nm and 80 respectively [154].
Polyethyleneimine (PEI) also used a material for biomedical applications. The cubic-shaped Fe3O4/PEI nanoparticles with the size
of 20 nm [150] and 50 nm [151] were prepared from KNO3 and FeSO4. Next, Fe3O4/PEI suspension was stirred and sonicated with
Au nanoparticles. The Au nanoparticles were produced by HAuCl4 including NaBH4 and reduction of sodium citrate. The Au na-
noshell was grown by a reduction of HAuCl4 in presence of NH2OH.HCl [150,151]. These nanoparticles that were synthesized during
314
this method showed good monodispersity and displayed size distribution 30 ± 5 [150].
Another important glue material is Polyaniline (PANI). Fe3O4 covered by PANI was proved to be paramagnetic thus, maybe a
perspective material to be used for several biomedical applications such as biosensors, drug delivery, enzyme immobilization, cancer
diagnosis and nucleic acid extraction [158]. In the work reported by Xuan et al, Fe3O4 nanoparticles were prepared via solvothermal
techniques and then melted into the water with a certain amount of aniline and HCl and then the mixture was shaken around for 12
hours. Next, Fe3O4/PANI sonicated with acetic acid would induce positive charges on the Fe3O4/PANI surface. Under the sonication,
Au seeds immobilized over Fe3O4/PANI nanoparticles surface because of the electrostatic attraction. Eventually, Au nanoshell has
formed by reduction with NaBH4 as a reducing agent thus the diameter of core Fe3O4 was 170 nm and the thickness of Au nanoshell
was 3 nm [152].
4. Surface modification
The modification of Fe3O4 nanoparticles surface with organic or inorganic materials can provide biocompatible nanoparticles for
the biomedical application. Coating Fe3O4 nanoparticles with inorganic materials such as gold and silica nanoparticles gave them
many advantages including, high stability and ability to bind biological molecules to the surface of Fe3O4 nanoparticles. On the other
hand, if hydrophobic Fe3O4 nanoparticles are coated with organic materials (hydrophilic polymers) such as chitosan, Polyethylene
glycol (PEG), Polyvinyl Alcohol (PVA), and Polyvinylpyrrolidone (PVP), the agglomeration of the iron oxide nanoparticles can mostly
be avoided.
4.1. Inorganic coating
4.1.1. Gold
Gold is an inorganic coating to implement functionality and improve the stability of magnetic nanoparticles in aqueous disper-
sions. Au coating has a unique feature called surface plasmonic resonance (SPR) which provides optical properties. Besides, the
coating with Au nanoparticles can also promote organic conjugation via Au-S chemistry. Fe3O4 coated with Au has been reported by
several authors [138,159,160]. The coating process is obtained by reducing the Au precursor in the existence of iron oxide nano-
particles. The experimental conditions differ according to the characteristics of the Fe3O4 nanoparticle like size, shape, surface
chemistry and the solubility, etc. Here we introduce some brief examples.
Xu et al. reported that magnetic Fe3O4/Au core/shell nanoparticles can be synthesized by reducing HAuCl4 at room temperature.
However, the work also indicates that the coating process of Au nanoparticles to cover the surface of Fe3O4 is difficult because of the
incompatible chemistry involved. Furthermore, The rapid reduction of HAuCl4 will lead to growth of Au nanoparticles rather than of
a coating shell. To prevent the rapid reduction, the process utilizes oleylamine as a moderate reduction agent in a chloroform solution
to slowly reduce HAuCl4 of Fe3O4 nanoparticles. Additionally, chloroform is a strong solvent and uses as a surfactant that may help
the desorption of oleylamine from the surface of Fe3O4 nanoparticles. Fe3O4/Au core/shell nanoparticles were soluble in a nonpolar
solvent due to an oleylamine still capped at the surface. To make them water soluble, Fe3O4/Au core/shell nanoparticles were dried
and mixed with cetyltrimethylammonium bromide (CTAB) and sodium citrate. The negative charge on the surface of the Au na-
noshell is due to the surface that may absorb the sodium citrate, which further led double-layer structure with the capping CTAB and
a powerful capping can be achieved to replace oleylamine. Under the reducing condition, the shell thickness Au depends on the ratio
of HAuCl4. This method not only to protect Fe3O4 from environmental corrosion but also able to manipulate and improve SPR
properties of the core/shell nanoparticles [138].
Zhong et al. reported another method to synthesis Fe3O4/Au core/shell [161]. The method includes Au (Ac)3 as a precursor with
temperature ranged 180-190°C in the existence of Fe3O4 nanoparticles, which used the reducing agent such as 1,2-hexadecandediol
and surfactants like oleylamine and oleic acid. At high heating temperature, the process of adsorption of oleic acid and oleylamine is
facilitated from Fe3O4 nanoparticles surface. This method employed a centrifuge to select the proper size and separated the small-
sized and large-sized core/shell nanoparticles and uncoated Fe3O4 nanoparticles. In addition, this method can control a combination
of thermally activated desorption of the capping layer and deposition of Au on the bare Fe3O4 surface, and re-encapsulation of the Au
surface by the capping agent. The shell thickness of Au nanoparticles was determined by TEM analysis [162]. After coating, the thiol
inter-particle was used to produce thin Fe3O4/Au core/shell nanoparticles.
Sheng-Nan et al also reported Au/Fe3O4 core/shell nanoparticles can be synthesize by co-precipitation method [162], Fe3O4
nanoparticles by this method usually their surfaces are full of in OH groups and water-soluble. The chemical surface such as Au or
other metal have difficulty in using for coating; therefore, it is necessary to modify by employ the organic inkers like (3-aminopropyl)
triethoxysilane (APTES). Also, a small amount of nitric acid HNO3 was also employed to make functionalized Au surface positively
charged. The mixture of APTES functionalized Fe3O4 nanoparticles, sodium citrate and HAuCl4 were sonicated and finally appeared
in Au coated Fe3O4.
4.1.2. Silica
Silica (SiO2) has been employed as an inorganic coating material for nanoparticle surface modification in the colloid system
[163–169]. Usually, the silica shell over the surface of Fe3O4 nanoparticles provides protection against toxicity, prevent the ag-
gregation of Fe3O4 nanoparticles in liquid and improve the chemical stability [170]. There are two different ways for the stability of
silica coatings over Fe3O4 nanoparticles [171]. Firstly, protection of the dipole interaction with the shell of silica secondly since silica
is negatively charged so it enhances the Coulomb repulsion of Fe3O4. The product is formed of Fe3O4 particles coated with silicon and
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Fig. 6. Preparation of Fe3O4/SiO2 core/shell nanoparticles [188].
its diameter 300 nm has been examined in the clinic by oral administration, they found it extremely improves the diagnosis of organ
boundaries, like lymph nodes and uterus [172–174].
In this review article, three strategies to create magnetic silica nanospheres will be presented. The first strategy depended on the
famous Stöber process, which states silica was produced in situ by condensation and hydrolysis of sol-gel precursors like tetraethyl
orthosilicate (TEOS) (Fig. 6) [175–179]. Xiong et al. have recorded silica colloids filled with SPIONs by this process have been
recorded [180]. This study revealed that there are two key factors to determine the final size of the silica colloids type of solvent and
the other is the concentration of Fe3O4 nanoparticles. The second strategy implicates a deposition of silica from the silicic acid
solution [181,182]. Several researchers have demonstrated the silica acid seems to be more effective than TEOS method in covering
Fe3O4 surface [183]. This method is easy and the particle size can be controlled by varying the ratio of Fe3O4 or SiO2 [184]. The third
strategy was about an emulsion way, in which micelle or inverse micelle are used to limit and control the coating of silica wherein the
separation of core/shell nanoparticles from the surfactant associated with an emulsion system [176,185,186]. For instance, Yang
et al. have employed this technique in the preparation of silica-coated SPIONs with monodisperse and increased the entrapment of
biological molecules in the nanoparticles [173].
Tartaj et al. used a pyrolysis method for coating magnetic sphere aerosol by silica [187, 188]. Gao et al. used seeds hydrophilic
Fe3O4 nanoparticles with size 20 nm used to prepare Fe3O4/SiO2 core/shell nanoparticles and the thickness of a SiO2 shell may be
tuned from 12.5 to 45 nm by varying the experimental conditions.
4.2. Organic coating
4.2.1. Chitosan
Chitosan is a biopolymer that has immense structural opportunities for mechanical and chemical modifications to produce novel
features, application and functions, especially in the biomedical section. It is hydrophilic, non-toxic, non-antigenic, biodegradable
and biocompatible polymer [189]. These days, the synthesizing of Fe3O4 nanoparticles encapsulated within chitosan are of prominent
importance [190,191]. Due to the presence of hydroxyl and amino on the chitosan would quickly form complexes with Fe3O4 surface
and making them stable, hydrophilic and biocompatible. The positive charge of amino groups could interact with a negative charge of
nucleic acids for MRI and therapeutic gene delivery [192,193].
Moreover, the use of chitosan would facilitate the flow of particles across cellular barriers as well as opening up a narrow junction
between epithelial cells [194,195]. Until now, this polymer has been used for coating SPIONs to produce an excellent contrast agent
for MRI [194,196–199]. Hong et al. synthesized chitosan-coated ferrite nanoparticles to be studied as a contrast agent for MRI [200].
The amino groups of chitosan (–NH2) were tied to the particles whereas the hydroxyl groups (–OH) remain untied. Consequently,
these kinds of particles have slightly positively charged. Due to the existence of Coulomb repulsion between the positive charge
particles and the absence of surface or organic solvents in an aqueous solution of coated particles, the solution will remain suspended
in a colloidal state. Kim et al. used the sonochemical technique to produce SPIONs. Kim and their group prepared ferrofluids as a
contrast agent for MRI. The nanoparticles' surface was coated with a surfactant such as oleic acid and then dispersing these particles
in the chitosan [201]. These spherical particles still retained the superparamagnetic behavior at a size of 15 nm in diameter. Mi-
crospheres composed of superparamagnetic iron oxide nanoparticles and chitosan were improved as a novel MRI-detectable embolic
material. Furthermore, Lee et al. have successfully synthesized 15 nm size spherical shaped SPIONs by employing the sonochemistry
process and then suspended nanoparticles within amino group chitosan to prepare a ferrofluid [202], where SPIONs/chitosan mi-
crospheres exhibited a strong improvement in MRI contrast like as ferrofluid in vitro.
4.2.2. Polyethylene Glycol (PEG)

PEG is a water-soluble and biocompatible polymer used in numerous applications in medicine. Many studies have been recorded
the utility of PEG [203–210]. It is working to increase the biocompatibility of blood circulation and iron oxide dispersions [211–213].
PEG acts as a suitable spacer for the linking of different biomolecules [214, 215]. Furthermore, when the targeting ligands, such as
antibody or protein are attached, the SPIONs accumulation is more precise to the region of concern, thereby saving normal tissues
[216–218]. There are a few problems that needed to be addressed for active drug release toward the target site. The drugs are
normally physically associated with the nanoparticle surface, and then they can be immediately released upon injection before
touching the target. Eventually, only the small part of the drug will approach its final destination. The second problem-based on the
coating on the particles may be digested under cytosolic conditions through displaying the particles to the cells then these particles
aggregate and cause improper conditions for cell survival. These reported problems can be avoided by using Fe3O4 nanoparticles
coated with (ethylene glycol)-co-fumarate (PEGF) that synthesized by Mahmoudi et al. [219].
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Recently, novel SPIONs coated with polymerized PEGylated bi-layers were prepared [220]. Different approaches to coating were
formed to provide ultra-small particles (20–35 nm) and small particles (60–100 nm). Kumagai et al. have mentioned an easy way to
prepare PEG-coated Fe3O4 nanoparticles through hydrolysis of (FeCl3.6H2O) in water and consequent treatment with PEG-poly
(aspartic acid) [221]. The nanoparticles with PEG-coated on their surface exhibited high stability and solubility in aqueous solution
and also in the physiological saline.
4.2.3. Polyvinyl Alcohol (PVA)

PVA is a biopolymer that widely used in medical applications such as drug delivery, ophthalmic materials and tendon repair
[222–224]. The particle surface coated with PVA showed good monodispersity and prevents the agglomeration of particles
[225–227]. PVA advantages are cell adhesion, possess high biocompatibility and resist protein adsorption [228]. Therefore, PVA can
be a good water-soluble and biocompatible material for coating over SPIONs [229]. Kayal et al. reported that coated SPIONs with
varying proportions of PVA and used as anti-cancer for drug delivery [230]. SPIONs coated with PVA, amino-functionalized PVA
(amino-PVA) and thiol-functionalized PVA have been reported [231] and tested these various functionalized PVAs with human
melanoma cells. To produce a more stable dispersion, the surface of nanoparticles can modify with PVA through precipitation the
iron salt in the PVA solution [232]. These researchers propose that PVA binds the surface of Fe3O4 by employing FTIR absorbance
shifts.
4.2.4. Poly vinyl pyrrolidone (PVP)

PVP is a water-soluble polymer that has been widely used in different biomedical applications because it possesses several
important properties such as neutral charge, aqueous solubility and biocompatibility [233,234]. Most of the previous studies showed
the PVP coated was obtained by covalent interaction and thus increased the stability of SPIONs in physiological media [235]. PVP-
coated Fe3O4 have been synthesized to esteem their efficacy as an MRI contrast agent [236]. PVP-coated SPIONs in one-step by
thermal decomposition technique was synthesized. Besides its water-solubility, PVP also can be soluble in different solutions in-
cluding saline, PBS and serum. According to the MRI contrast agent, the T2-weighted results demonstrated that PVP coated SPIONs
were a little better than Feridex (ferumoxides injectable solution). The PVP coated SPIONs retain a high magnetic moment that results
in high relaxivity. PVP-SPIONs and Feridex were compared as an MRI contrast agent. They found that until the low concentration of
Fe, The PVP-coated SPIONs showed improvement a higher negative contrast than Feridex. Due to the high solubility and mono-
dispersity of PVP-SPIONs in the buffer solution, the PVP-SPIONs can perform a bolus injection without the filteration, unlike Feridex.
5. Applications of Fe3O4/Au nanocomposites
In this part, selected applications of Fe3O4/Au nanocomposites material including MRI, CT scan, drug delivery, biosensors and
hyperthermia (Fig. 7), are discussed.
5.1. Magnetic resonance imaging (MRI)
MRI is a noninvasive technique utilized for diagnostic imaging human in vivo. It provides enhanced monitor ability for tracking
cells with high contrasting and remains cell contains a large amount of Fe3O4 nanoparticles [237]. MRI technique is preferred over
the other techniques like positron emission tomography (PET), single-photon emission computed tomography (SPECT) and computed
X-ray tomography (CT) for several reasons such as deep penetration of magnetic field, high-resolution for anatomic images and
contrast agents is non-ionizing [238, 239]. It is based on the behavior of nuclear magnetization of the proton particles that exist in the
body. Upon the application of a magnetic field, longitudinal magnetism will be produced by spin the protons in the body through a
parallel motion and align to the direction of the magnetic field. Under the radio frequency (RF) pules, inducing transverse magne-
tization by spin, the protons align the antiparallel direction of the magnetic field. When the RF pulses are turned off, the excited
protons will emit energy when return to the original state. This relaxation procedure happens in two independent processes firstly
longitudinal relaxation (T1-recovery) and the second is transverse relaxation (T2-decay).
The contrast agent (CA) shown images brighter over T1 and darker images through T2. Recently, the previous study demonstrated
that SPIONs have been broadly utilized as T2 based MRI contrast-enhancing agents because of its high relaxivity, excellent contrast
impact, susceptibility and high saturation magnetization, biocompatibility, low cost, and non-toxicity. Au nanoparticles are good
contrast agents for bioimaging due to their absorption properties, biocompatibility and surface functionalization, combining Au
encapsulates SPIONs and makes it a highly efficient contrast agent. SPIONs@Au nanocomposites are attractive materials that employ
for medical areas because of their theranostic features involving MRI and CT, etc. These nanocomposites can be dumbbell-shaped
[240], core/shell [241–244] and flower-shaped [245,246], as expected, the structures of nanocomposites effect on the transverse
relaxivities [241–247]. In the case of MRI response, the transverse (r2) relaxivities of Fe3O4/Au nanocomposites are relatively lower
compared with other nanostructure [241, 242,244] such as dumbbell nanocomposites due to shielding impact on an embed the core
of Fe3O4 inside an Au shell [248]. In MRI contrast, the Fe3O4/Au core/shell nanocomposites display relatively higher transverse
relaxivity (r2) values [243].
5.2. Computed tomography (CT)
CT is one of the most widely used tools in hospitals for diagnosis and treatment of cancer. CT scan is an X-ray strategy that
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Fig. 7. Schematic representation biomedical application of Fe3O4/Au nanocomposite.
produces cross-sectional images 3D by computer. Which is based on the absorption of X-ray when it passes into the tissues. Contrast
images of the anatomical structures have been produced through various tissues by differentiation X-ray attenuation. In principle, a
density of the electron in the tissues and atomic number is the critical coefficient for X-ray attenuation. Recently, Au nanoparticles
have been suggested as CT contrast agents because of the high atomic number and density of the electron [249]. Jeong et al. in-
troduced a proper combination of Fe3O4 and Au as a dual-modality for (CT/MR) imaging [248]. Fe3O4/Au nanoparticles like
strawberry shape have been used as CA in the dual-modality (CT/MR) for precise detection of liver diseases [250]. The presence of Au
layers showed high CT attenuation whereas the signal MRI T2 lower than normal SPIONs because of the embedded Fe3O4 core. On the
other hand, Fe3O4/Au dumbbell nanocomposite is introduced and serve as contrast agents dual (CT/MRI) without lowering signal
intensity T2 in vivo MRI study. Hounsfield unit (HU) of the dumbbell nanocomposites displays higher attenuation (723 at 100 mM
Au) compared to pure Au nanoparticles (528 at 100 Mm Au) with same concentrations of Au [251].
In vitro studies showed that the core@shell shell (CSs) revealed CT contrast improvement, which showed that the CSs of Fe3O4/
Au potentially used in dual-modality (CT/MRI) as contrast agents (CAs), good biocompatibility and bearing less toxicity among cell
lines. The composite of CS revealed that a good X-ray attenuation property and a relatively high of r2 relaxivity, through data of CT
and MRI. Cai et al. have been developed a facile assembly to the preparation Fe3O4/Au nanocomposites for dual-modality (CT/MR)
imaging [252]. The increase in Fe concentration showed the signal of cells got brighter through CT, whereas the value of T2 in MRI
decreases.
5.3. Drug delivery
Chemotherapy is still one of the most popular way to treat since it only depends on the circulatory system to deliver drugs to
cancer cells even though it lacks the specificity on the tumor. As such, this method increases the amount of toxicity that affects non-
diseased tissues by introducing a lot of drugs into the body of the patient. Because of these serious complications on the patient,
targeted drug delivery that provides treatment for the tumor area has brought significant attention to the replacement of che-
motherapy [253]. In drug delivery research, Fe3O4 nanoparticle is preferred over the other targeting techniques due to its ability to
combine with other methods such as electric fields and ultrasound. The Fe3O4 nanoparticles are modified with a proper bio-coating
which enables surface functionalization, such that the drug is attached to it. Under the external guide from the magnetic field, these
small particles are delivered to the tumor site. Magnetically targeted drug delivery (MTD) is a useful treatment of malignant cells by
an accumulation of chemotherapeutic representatives at the target site. Many different factors play an important role in MTD such as
biocompatibility of magnetic nanoparticles, size, shape and stability in physiological conditions [254–258]. The forming a shell of Au
nanoparticles for magnetic nanoparticles would be highly desirable of magnetic nanoparticles in MTD due to stability and
318
biocompatibility, bio-conjugation and ease of preparation [145,257,259]. SPIONs/Au CSs packed doxorubicin (DOx) as an anti-
cancer drug were studied as a possible cancer therapy by combining both drug delivery and hyperthermia [258].
Various conditions such as oscillatory magnetic fields, temperature and different pH conditions have been studied for drug release
efficacy. It was found that acidic pH and oscillating field conditions improved the effective release of drugs while they were not
affected by high temperatures. The drug release study showed that pH level 5.5 records a higher drug release than the other levels.
SPIONs/Au–Cyst–DOx with non-toxic behavior has been proved appropriateness for drug delivery. Karamipour et al. manufactured
Fe3O4/Au CSs conjugate with folic acid by using linker such L-cysteine [Fe3O4/Au/Cys-Folate] to targeting folate receptor that exists
on the top of cancerous cells [254]. The attachment between Fe3O4/Au CSs and L-cysteine and folic acid confirmed by FTIR and UV-
visible results. The advantage of Fe3O4/Au CSs for cancer treatment in the MTD as a DOx carrier has been reported recently by Elbialy
et al. [145]. In their work, the Fe3O4/Au CSs is functionalized to include anti-cancer drug DOx packed over thiol-terminated poly-
ethylene glycol for bio-compatibility improvement.
5.4. Biosensors
The biosensor is a device that captures a biological signal and converts it into an electrical signal that can be detect biological
molecules such microorganisms, proteins and DNA [260]. Several metal nanoparticles and specially Fe3O4/Au core/shell CSs have
been extensively studied as biosensors such enzyme-based sensors, immunosensors and DNA sensors due to its special magnetic and
optical characteristics, easily tuned surfaces and biocompatibility, further utilize thiol chemistry to attach the molecules on Au
nanoparticles [134]. These heterogeneous materials, Fe3O4/Au, which include two nanocrystals, have recently attracted significant
attention for fast and sensitive detection of the tumors markers. The catalytic properties and surface area of the magnetic cores and
mediators also make them appropriately suitable as electrochemical sensors. The presence of Au nanoparticles onto SPIONs improves
their catalytic activity and the sensitivity in biosensors compared to that of single-component nanoparticles. For DNA sensing, Stoeva
et al. have been demonstrated a composite structure of three layers SiO2/Fe3O4/Au nanoparticles [261]. These nanoparticles with its
top surface-functionalized (with two different types 3ʹ- and 5ʹ- thiol of DNA modification) is now ready for complementary hy-
bridization.
5.5. Hyperthermia
Hyperthermia is considered one of the oldest ways to treat cancerous diseases with fewer side effects compared to radiation
therapy and chemotherapy. It is referred to as using high temperatures ranged from 42-48°C to kill cancer cells. Hyperthermia can be
located within a specific region or whole body region [262]. Tumor cells are higher sensitive exposure to heating than non-diseased
cells more specific, the exposure to high temperature either result in the death of cells or susceptible to radiation therapy or che-
motherapy. The increase of temperature above 42°C leads to cell apoptosis and the cell necrosis occurs above 46°C. For apoptosis,
caspase-9 that results in cell death will induce via pro-apoptosis proteins. The Radio frequency (RF) wave, microwave and laser can
induce hyperthermia in the body region by the introduction of a chemical or by using nanoparticles [262]. Hyperthermia mechanisms
for magnetic and Au nanoparticles can be classified into two general categories: first the magnetically induced hyperthermia for
magnetic nanoparticles and the second is photoinduced hyperthermia for Au nanoparticles [263]. Shete et al. has demonstrated the
effectiveness of combined material as a core/shell nanoparticle format. A combination of both materials will open a new door and
possibilities in medical and health care applications.
6. Conclusions
The review shows the most popular wet chemical and efficient synthesis approaches for Fe3O4 nanoparticles such as co-pre-
cipitation, electrochemical, hydrothermal, microemulsion, sol-gel, solvothermal, sonication and thermal. Bi-layer and multilayer
architectures of Fe3O4/Au and Fe3O4/glue/Au nanocomposite materials have been effectively synthesized. Nevertheless, efforts
should be made to synthesize novel monodisperse Fe3O4/Au core/shell and Fe3O4/glue/Au core/glue/Au nanocomposites structures
to overcome some of the synthesis challenges. While the modifications will reduce the physiochemical properties of the core material
of Fe3O4/Au and Fe3O4/glue/Au nanocomposites, the intrinsic modularity of the synthesis processes should be ensured to enable the
fast and uninhibited interaction between several similar nanocomposites and other metal/metals oxide, to suit the requirements
(surface area, specific functions and morphology) of any application. It would be stimulating in future review to investigate various
novel morphologies and structures of these materials in advanced bio-medical applications.
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.
Acknowledgment
The authors would like to thank USM Bridging-Grant 304.PFIZIK.6316530 for the funding and support for this research work.
319
Financial support and sponsorship
Nil.
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Chinese Journal of Physics 64 (2020) 305–325

Contents lists available at ScienceDirect

Chinese Journal of Physics

Synthesis and coating methods of biocompatible iron oxide/gold

with suitable materials that can enable biocompatibility [12].

2. Wet chemical methods for the synthesis of magnetite nanoparticles

2.1. Co-precipitation method

2.2. Electrochemical method

2.3. Hydrothermal method

Hydrolysis: Mn+ +nH2O → M(OH)n + n H+ (1)

Dehydration: M(OH)n → MOn/2 + n/2 H2O (2)

Fig. 2. Shows the formation of nanoparticles via w/o microemulsions [70].

2.4. Microemulsions and reverse micelles method

2.5. Sol-gel method

2.6. Solvothermal method

2.7. Sonication method

2.8. Thermal decomposition method

3. Synthesis of Fe3O4/Au Core/shell nanocomposite

3.1. Synthesis of a Fe3O4 bi-layer structure

Fig. 4. Schematic representation of two approaches for synthesis Au coated Fe3O4.

Fe3O4/Au I Co-precipitation Reduction by citrate 20 22 (2 nm gold shell) T2 in MRI [135]

3.2. Synthesis Fe3O4/glue/Au multilayer

4.1. Inorganic coating

Fig. 6. Preparation of Fe3O4/SiO2 core/shell nanoparticles [188].

4.2. Organic coating

4.2.2. Polyethylene Glycol (PEG)

4.2.3. Polyvinyl Alcohol (PVA)

4.2.4. Poly vinyl pyrrolidone (PVP)

5. Applications of Fe3O4/Au nanocomposites

5.1. Magnetic resonance imaging (MRI)

5.2. Computed tomography (CT)

Fig. 7. Schematic representation biomedical application of Fe3O4/Au nanocomposite.

5.3. Drug delivery

Declaration of Competing Interest

Financial support and sponsorship

performance anode in lithium ion batteries, Chem. Commun. (2009) 7360–7362.

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