Applied Surface Science Advances 6 (2021) 100145

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Applied Surface Science Advances

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Spinel ferrites nanoparticles: Synthesis methods and application in

heterogeneous Fenton oxidation of organic pollutants – A review
Amal SOUFI a, Hind HAJJAOUI a, Rachid ELMOUBARKI a, Mohamed ABDENNOURI a,
Samir QOURZAL b, Noureddine BARKA a, *
a
Sultan Moulay Slimane University of Beni Mellal, Research Group in Environmental Sciences and Applied Materials (SEMA), FP Khouribga, Morocco
b
Equipe de Catalyse et Environnement, Département de Chimie, Faculté des Sciences, Université Ibn Zohr, B.P. 8106 Cité Dakhla, Agadir, Morocco

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

Keywords: Heterogeneous Fenton-like oxidation is one of the advanced oxidation processes (AOPs) that can successfully
Fenton-like remove a large number of pollutants from water. Among various materials used as catalysts in this process, spinel
Oxidation ferrite nanoparticles (SFs) have received increasing attention in recent years because of their unique physico­
Metal ferrites
chemical properties, low-cost, good catalytic activity and interesting bandgap. In the same vein, their magnetic
Emerging contaminants
properties allow them to be easily, rapidly and inexpensively separated from the reaction medium. The present
Recyclable catalyst
review highlights the unique structure and properties of different spinel ferrite nanoparticles, their synthesis
approaches and their applications as a catalyst in heterogeneous Fenton-like and photo-Fenton-like oxidation. It
was demonstrated that MFe2O4 have unlimited ability as catalysts in both heterogeneous Fenton-like and photo-
Fenton-like oxidation. Thus, it can be deduced that their catalytic activity depends on the nature of divalent
metal M, synthesis method, annealing temperature, pollutant nature and concentration, H2O2 concentration, pH,
temperature and light source for photo-Fenton-like oxidation.

1. Introduction
Nowadays, the pollution of the global water cycle with persistent
organic contaminants remains one of the major challenges of the 21st
century [1]. Polluted water significantly affects human health, envi­
ronment, aquatic ecosystems, economic and social well-being of society
[2]. Several pollutants, such as industrial dyes, pharmaceuticals, agro­
chemicals, petroleum refinery plants and leachate from landfill have
been widely detected in wastewaters. These various contaminants are
highly resistant, toxic and have caused serious issues to the ecosystem
even at low concentrations [3,4]. Therefore, there is a need to remove
these persistent pollutants from effluents before discharging them in
receiving aquatic systems.
Various methods have been developed and designed to deal with
contaminated water, such as adsorption, sedimentation, coagulation,
flocculation, membrane filtration, distillation, ion exchange, crystalli­
zation, ultrafiltration, reverse osmosis, electrodialysis and electrolysis.
However, most of these methods are not capable to completely degrade
the pollutants in wastewater or generate secondary polluted compounds
that cannot be separated after treatment [5]. In the last decades, AOPs
have proven to be highly effective treatment processes due to their high
ability to completely mineralize the pollutants without the addition of
hazardous substances [6]. These processes are based generally on the
generation of the highly active oxidizing hydroxyl radicals species (HO•,
E0 = 2.80 V/SHE) which is the key factor for effective decomposition of
organic pollutants [7,8]. Several methods are available for generating
HO• radicals, including UV-based processes (UV/O3/H2O2), chemical
oxidation processes (O3/H2O2), photocatalytic oxidation (UV/Solar in
the presence of semiconductors such as TiO2 and ZnO etc.), Fenton and
photo-Fenton processes (Fe2+/H2O2/UV), etc.
Among AOPs, Fenton-type reactions have been identified as effective
methods which produce hydroxyl radicals by the reaction between iron
salts and hydrogen peroxide as shown in Eqs. (1) and (2).
H2 O2 + Fe2+ →Fe3+ + OH − + HO⋅ (1)
H2 O2 + Fe3+ →Fe2+ + H + + HO⋅2 (2)
(Known as Fenton-like reaction)
The advantages of these processes are the simplicity of equipment
and the mild operating conditions usually employed as well as short

* Corresponding author.
E-mail address: barkanoureddine@yahoo.fr (N. BARKA).

https://doi.org/10.1016/j.apsadv.2021.100145
Received 9 March 2021; Received in revised form 27 June 2021; Accepted 12 August 2021
Available online 19 August 2021
2666-5239/© 2021 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
A. SOUFI et al.
reaction time, the absence of mass transfer limitations, high degradation
efficiency, general applicability, no selectivity with organic and inor­
ganic compounds, rapid degradation and mineralization [9,10]. More­
over, the use of hydrogen peroxide is safe and easy to handle, and poses
no lasting threat to the environment as it decomposes easily into water
and oxygen. Likewise, iron is inexpensive, safe and environmentally
friendly [11].
The industrial application of classical Fenton process based on ho­
mogeneous ferrous or ferric salts usually suffers several drawbacks such
as formation of sludge at the end of the process, narrow pH range, be­
tween 2 and 4, the production of iron-contained sludge and the catalyst
deactivation by some iron complexing agents such as phosphate anions
and some intermediate oxidation products. In addition, the catalysts
cannot be recycled which increases the cost for the treatment of real
wastewater. Despite major drawbacks encountered by traditional ho­
mogeneous Fenton in the last decade, Fenton process still receives much
attention with more emphasis on heterogeneous processes, in which
solid iron-based catalysts were used instead of soluble iron salts. As can
be seen in Fig. 1, the number of publications devoted to this process is in
steady increase.
Among various materials applied as heterogeneous Fenton catalysts,
nanomaterials with spinel structure such as transition metal ferrites
MFe2O4 (M = Fe, Co, Ni, Mn, Mg, Cu and Zn, etc.) have attracted an
increasing attention, due to their high natural abundance, low cost, good
catalytic activity, large surface area, selectivity, surface oxygen mobility
property, electrical conductivity, high thermal, mechanical and chemi­
cal stabilities. Furthermore, the magnetic properties of ferrites permit
their easy, fast and inexpensive separation from the reaction medium
[12,13]. All of these characteristics make ferrites better catalysts not
only in Fenton reactions but also in heterogeneous advanced oxidation
processes compared to other iron oxides or conventional Fe-supported
catalysts.
2. Spinel ferrites
2.1. Structure
The structure of SFs as possessed for MgAl2O4 was first determined
by Bragg and Nishikawa in 1915. The general structural formula of a
spinel ferrite can be written as MFe2O4, where M stands for the divalent
metal ion like, Fe, Co, Ni, Mn, Mg, Cu and Zn, etc. or a combination of
these ions. The spinel structure belongs to space group Fd3m (JCPDS:
Fig. 1. Evolution of the number of scientific papers devoted to the applications
of heterogeneous Fenton processes. Source: Web of Science; Topic: “Heteroge­
neous Fenton” and “Catalytic Wet Peroxide Oxidation”; Searching time: 15
June 2021.
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Applied Surface Science Advances 6 (2021) 100145
22–1086) [14]. The unit cell of spinel ferrite (Fig. 2) is face-centered
cubic (f.c.c) with eight formula units per unit cell (M8Fe16O32) [15].
In one unit cell of ferrite there are 96 interstices (64 tetrahedral and 32
octahedral) exist between the close packing of oxygen atoms [12]. Only
8 tetrahedral and 16 octahedral positions are occupied by the cations
[13]. They are called (A) and (B) site respectively. The distribution of
each metal depends on its affinity for the both positions. This affinity
depends on the stabilization energy, the ion rays of the specification, the
size of the interstices, the synthesis method and the conditions employed
during the synthesis time [16]. The type and distribution of cations at
tetrahedral and octahedral sites have a significant implication on both
the physical and chemical properties of ferrite nanoparticles [16].
2.2. Classifications
Based on the distribution of cations at the tetrahedral (A) and octa­
hedral (B) sites, SFs have been classified into three categories. This
classification is based on the degree of inversion, x, defined as the
fraction of M2+ ions occupying octahedral sites, according to
3+ 3+
[M2+ 2+
1− x Fex ](A) [Fe2− x Mx ](B) [17], generally used to characterize the
cationic disorder. When x = 0, it is called normal spinel; when x = 1, it is
called an inverse spinel; when 0<x<1, it is called mixed spinel. In
normal SFs, the divalent cations M2+occupy tetrahedral (A) sites while
the trivalent cations Fe3+ are on octahedral (B) site. The structural for­
mula of such ferrites is [M2+](A) [Fe23+](B)O42− , examples: ZnFe2O4,
CdFe2O4 [18,19]. In inverse SFs, the divalent cations M2+occupy octa­
hedral (B) sites while one half of the trivalent cations Fe3+ are placed in
(A) sites and another half in (B) sites. The structural formula of these
ferrites is [Fe3+](A) [M2+Fe3+](B)O42− . Examples: Fe3O4, CoFe2O4 and
NiFe2O4 [20], CuFe2O4 [21]. MgFe2O4 [22]. In the case of mixed spinel
ferrites, the divalent cations M2+ and the trivalent cations Fe3+ ions are
distributed at both tetrahedral (A) site and octahedral (B) site. Examples:
MnFe2O4 [23]. It can be noted that, x depends on the method of prep­
aration and the nature of the constituents of the ferrites. For example,
CuFe2O4 can form either inverse or mixed spinel structure type,
depending on the conditions employed for the synthesis [24].
2.3. Properties
SFs have attracted considerable interest among researchers owing to
their unique electrical, dielectric, electronic, mechanical, magnetic,
optical and catalytic properties [25]. The SFs are unique materials
exhibiting ferrimagnetic and semiconductor properties and can be
considered as magnetic semiconductors [26]. They possess special
Fig. 2. Unit cell structure of spinel ferrite showing tetrahedral and octahe­
dral sites.
A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

physicochemical properties including high Curie temperature, large

magneto crystalline anisotropy, good thermal stability, and modest
chemical composition. In addition, they have excellent magnetic char­
acteristics, tunable size and shape, high specific surface area, surface
active sites, high chemical stability and also the ease with which they
can be modified or functionalized [27]. These properties depend on the
nature of divalent cation in the spinel structure (besides Fe3+) and their
distribution at tetrahedral and octahedral sites, synthesis method, grain
size, morphology and annealing temperature, etc. [12,14].. Further­
more, SFs have been recently widely investigated in water treatment due
to their low cost, good catalytic activity, interesting bandgap, selec­
tivity, the capability to recover and reuse in further cycles without
remarkable loss of activity and the low toxicity [28]. Fig. 3 summarizes
some advantages of SFs nanoparticles.
Fig. 4. Different fields that utilize spinel ferrites. Source: Scopus; Topic: “Spinel
2.4. Applications Ferrite”; Searching time: 15 June 2021.

The potential structural, electrical and magnetic properties of SFs
offered their application in various fields as shown in Fig. 4. In this re­
gard, they have been widely used as magnetic materials [29,30], as
adsorbent for the removal of heavy metals [31,32] and dyes [33,34]
from water and wastewater, or as catalyst and photo-catalyst to remove
different pollutants [35,36]. Additionally, they could be used either as
contrast agents [37], hyperthermia [38,39], drug delivery and release
[40,41], as sensors/biosensors in biotechnological and medical appli­
cations, in electronic device, microwave device, electromagnetic
interference shielding and recording media [42–44].
3. Synthesis methods of spinel ferrites nanoparticles
Nowadays different routes are used for the preparation of SFs
including solid state, co-precipitation, sol-gel, hydrothermal, micro­
emulsion, solvothermal, template method, sono-chemical, electro­
chemical etc. Nevertheless, until now, there is no universal method of

Fig. 3. Different properties of spinel ferrites nanoparticles.

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A. SOUFI et al.
the synthesis of SFs nanoparticles and each of these synthesis methods
has its own advantages and disadvantages. Furthermore the
morphology, the structure and the properties of these magnetic ferrites
are strongly influenced by the preparation methodology used in their
synthesis and may influence the catalytic activity of these materials
when used as catalysts [16]. Thereby, the effect of the preparation
method on the catalytic activity is a very interesting subject.
3.1. Solid state
The mechanism of spinel ferrite formation by solid-state reactions
has been discussed by several researchers based on simple diffusion
couple involving the iron and metal salts. In this method, the required
composition is usually prepared from the appropriate amount of raw
mineral oxides or carbonates by crushing, grinding and milling. The
overall preparation process generally comprises four major steps; (1)
Preparing a mixture of desired composition, (2) Pre sintering the
mixture to form ferrite, (3) Converting the raw ferrite into powder and
pressing the powder, and (4) Sintering. This method suffers from un­
controlled stoichiometry, poor composition, chemical inhomogeneity,
contamination, coarser particle size, and introduction of impurities
during grinding and high annealing temperature. In this context, wet
chemical methods have emerged as savior and offer ferrite nanoparticles
with reproducible stoichiometric composition and desired microstruc­
tures [45].
3.2. Co-precipitation
The co-precipitation is one of the oldest synthesis methods to obtain
SFs. It’s the most convenient, economic, and less time-consuming that
has high mass production. It is frequently employed as it provides ma­
terials with uniform particle size [46]. The process involves addition of
stoichiometric amounts of desired aqueous metal salt solution with
continuous and vigorous stirring in an alkaline solution (NaOH or
NH4OH). The pH of the solution plays important role in the formation of
different types of nano-ferrite spinel and needs careful monitoring in
order to achieve high-quality materials [47]. Fig. 5 shows the schematic
diagram of experimental setup used in this method. A variety of SFs have
been synthesized by coprecipitation including CuFe2O4 [48], CoFe2O4
[49], MnFe2O4 [50], MgFe2O4 [51], etc.
Fig. 5. Flowchart for the synthesis of spinel ferrite by co-precipitation method.
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Applied Surface Science Advances 6 (2021) 100145
3.3. Sol-gel
Sol-gel process consists on the preparation of inorganic polymers or
ceramics from solution through a transformation from liquid precursors
to a colloidal solution (sol) and finally to a network structure called a gel
[52]. It’s a well–known and most popular method used to synthesize
nano-ferrites and their composites. Sol-gel is a rapid and inexpensive
process and yields highly pure and crystalline nano materials with ho­
mogeneous size distribution [53]. It’s usually recognized as sol-gel
auto-combustion, sol-gel autoignition, sol-gel self-combustion,
low-temperature self-combustion, auto-ignition or self-propagation, as
well as gel-thermal decomposition [54]. In this process, stoichiometric
amounts of metal precursors are dissolved in minimum amount of
distilled water followed by the addition of an appropriate organic fuel
(chelating/combustion agents), such as citric acid (C6H8O7), urea
(CH4N2O), glycine (C2H5NO2), ethylene glycol (C2H6O2), hydrazine
(N2H4), carbohydrazide (CH6N4O), alanine (C3H7NO2), acetic acid
(CH₃COOH) and acrylic acid (C3H4O2), hexamethylenetetramine
(C6H12N4), polyvinyl alcohol (C2H4O)n, etc. The pH of resultant solution
is then adjusted by adding dilute ammonia solution (NH4OH). Then the
solution is allowed to evaporate till gels are formed, which on contin­
uous heating undergo combustion to give a solid powder. The solid
powder is annealed in a furnace at various temperatures. Among these
fuels, citric acid is the most frequently used for the preparation of a large
variety of spinel ferrites. It is inexpensive and is a more effective com­
plexing agent than hydrazine and glycine in producing fine ferrite
powder with smaller particle size [55]. In general, a good fuel should
react non-violently, produce nontoxic gasses and act as a complexant for
metal ions [56]. The effectiveness and production of high quality fine
powder depends on the nature of fuel, fuel to oxidizer ratio, precursors’
concentration, pH, agitation, heating mechanism, annealing tempera­
ture and the preparation condition [57,58]. Fig. 6 represents a schematic
illustration for the synthesis of SFs by sol-gel technique. Over the last
decade, a variety of SFs have been synthesized by sol-gel method
including: MgFe2O4 [59], CuFe2O4 [60,61], ZnFe2O4 [62], NiFe2O4
[63], CaFe2O4 [64], CoFe2O4 [65], MnFe2O4 [66], etc.
3.4. Microemulsion
Microemulsions are isotropic and thermodynamically stable systems
A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Fig. 6. Flowchart for the synthesis of spinel ferrite by sol-gel method.

composed of two relatively immiscible liquids, and surfactant [67].
Microemulsion method yields nanoparticles with a narrow size distri­
bution and size control readily achievable by minor adjustments to the
synthesis conditions. This method involves three components; water, oil
and surfactant and enables to control various properties such as particle
size, geometry, morphology, homogeneity and surface area [68]. It
could be categorized into normal micelle methods [oil-in-water (o/w)]
and reverse micelle methods [water-in-oil (w/o)]. In both methods
surfactants are used and their concentration is above the critical micelle
concentration (CMC) [69]. The schematic diagram for the micro­
emulsion process is shown in Fig. 7. This process is known for being
eco-friendly and favorable at low temperature and reuse of surfactants
for several cycles during the synthesis and possibility of commercial
production. Nevertheless, the major disadvantage is the poor crystalline
nature of synthesized SFs, requirement of larger amounts of solvents and
high polydispersion due to the slower nucleation rate at low tempera­
ture [70]. Among the spinel ferrite synthesized by microemulsion
method we can mention: MFe2O4; M:Co, Ni and Zn [71], Mn–Zn ferrite

Fig. 7. A schematic representation of the synthesis of spinel ferrite nanoparticles using the reverse micelle method.

5
A. SOUFI et al.
[72], etc.
3.5. Solvo(hydro)thermal method
The solvothermal method (or hydrothermal if water is solvent) is one
of the most eco-friendly and promising synthesis methods which is
available and employs the usability of aqueous or non-aqueous solvents
for a better control of particle size distribution and morphology [70].
This method consists of the formation of uniform solution of the metal
salts followed by the addition of a base until basic pH is reached. The
resulting mixture is then transferred into an autoclave and treated at
140–220 ◦ C for many hours [73,74]. The heating temperature and time
dependents on the type of the target NPs [16]. The solid products were
collected with a magnet and washed separately with distilled water and
ethanol for several times and dried. Finally, the dried powders were
further sintered [75]. The mechanism involves the initial formation of
metal hydroxides, which are oxidized and converted into the crystalline
spinel ferrite due to the thermal treatment at high pressures. The
resulting NPs have high crystallinity and an acceptable narrow size
distribution. Particle size and shape of the nanoparticles can be opti­
mized by adjusting the reaction time, the reaction temperature, solvent
type, surfactant type, and precursor type [76]. A variety of SFs have
been synthesized by both hydrothermal method: ZnFe2O4 [77], NiFe2O4
[78], CuFe2O4 [79], MgFe2O4 [73] and solvothermal method: ZnFe2O4
[74], CuFe2O4 [79], MgFe2O4 [80], Fe3O4 [81], NiFe2O4 [82], CoFe2O4
[83], MnFe2O4 [84], etc.
3.6. Template method
Template synthesis is a relatively simple and easy procedure which
has made the fabrication of rather sophisticated nanomaterials. The
method is based on the simple but effective idea that the pores of a host
material can be used as a template to direct the growth of new materials.
The role of the template is twofold. First, it allows the reproduction of
the structure with the best possible reproducibility and plays the role of
a skeleton in order to organize the different functions of a device, the
active components, and the different interfaces [85]. The general route
for templated synthesis of nanostructured materials includes the
following steps: (1) template preparation, (2) directed synthesis of target
materials using the template, and (3) template removal (if necessary)
[86]. SFs synthesized by this method include MFe2O4 (M = Ni, Mg, Co)
[87], ZnFe2O4 [88], NiFe2O4 [89], MgFe2O4 [90], CoFe2O4 [91].
3.7. Sonochemical
Sono-chemical technique is relatively new, effective and compara­
tively easy method for the synthesis of ferrite nanoparticles without
using any toxic or hazardous and expensive chemicals [92]. This method
is advantageous for the synthesis of nanoparticles due to the facile
control of reaction conditions, good control of particle size distribution,
highly monodispersed nanoparticles, and very small nanoparticles [93].
Therefore, the temperature and the intensity of ultrasonic waves are
major factors which can have a direct impact on the particle size of SFs.
In sono-chemical synthesis, during ultrasound irradiation, sound waves
propagate through the liquid and at the same time microbubbles are
created, and SFs undergo in-situ calcination due to the induced
high-energy collisions between the particles. By means of ultra­
sonication, mixing at the atomic level can be achieved so that the for­
mation of crystalline phase is possible at relatively low temperatures.
Among the spinel ferrite synthesized by sono-chemical method we can
mention: CuFe2O4 [94], Co0.3Ni0.5Mn0.2EuxFe2− xO4 [95], MnFe2O4
[96], etc.
3.8. Electrochemical
An electrochemical synthesis can be basically interpreted by passing
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Applied Surface Science Advances 6 (2021) 100145
an electric current between two or more electrodes (anode and cathode)
located in an electrolyte. In this technique, the anode can be oxidized to
metal ion species in the electrolyte and the metal ion is later reduced to
metal by the cathode with the assistance of stabilizers [97]. The key
factors of this method are the current density, pH, electrolyte compo­
sition, electrode choice, applied cell potential, temperature, stirring and
distance between the electrodes which can significantly influence the
crystallinity and particle size of the product [98,99]. In general, elec­
trochemical synthesis method is simple, inexpensive, environmentally
friendly, and cost-effective [16]. Among the SFs synthesized by elec­
trochemical route we can mention: MnFe2O4 [100], Fe3O4 [101],
MFe2O4 (M = Fe, Mn, Co, Ni) [98], NiFe2O4 [102], CoFe2O4 [103], etc.
3.9. Other methods
Numerous other methods frequently employed for the synthesis of
SFs have been reported in the literature, including flame spray pyrolysis
[104], Laser ablation [105], microwave-assisted method [106], elec­
trospinning [107], and mechanical milling method [108].
3.10. Comparison of synthesis methods
The properties of SFs are strongly influenced by the preparation
methodology used in their synthesis. Each synthesis method has its own
advantages and disadvantages as shown in Table 1. Varma et al. [109]
reported that the particle size and magnetic properties of CoFe2O4
strongly depend on the method of preparation. Kaur et al. [51] fabri­
cated MgFe2O4 using different methods keeping uniform calcination
temperature and sintering time. Differences in crystallinity, surface area,
particle size and magnetic parameters of SFs nanoparticles synthesized
by different methods were observed. Furthermore, Kumar et al. [68]
found that the shape and size of different types of SFs nanoparticles
directly depend upon synthetic methods. Moreover, they reported that
the characteristics of different types of MFe2O4 are controlled by
different factors such as precursor composition, pH of solution and
annealing temperature. In other words, each method has its own char­
acteristics and the preparation methods can be selected according to the
needs of the application [110].
4. Magnetic properties
Depending upon the nature (magnetic or non-magnetic) and distri­
bution of cations at the tetrahedral (A) and octahedral (B) sites, SFs can
be classified into the following sex major groups: paramagnetic,
diamagnetic, ferrimagnetic, ferromagnetic, antiferromagnetic, and
superparamagnetic. Fig. 8. presents the major important magnetic
properties of spinel ferrites which are saturation magnetization (MS),
remnant magnetization (Mr) and coercivity (Hc). High saturation
magnetization (Ms), with negligible coercivity (Hc) symbolizes the
superparamagnetic properties of these materials which have a great
importance in water treatment. Superparamagnetism appears in small
ferromagnetic or ferrimagnetic nanoparticles, their diameter is below
3–50 nm, depending on the materials [111]. Nowadays, super­
paramagnetic nanoparticles is so famous because of the properties
possessed, where the nanoparticles are magnetized up to their saturation
magnetization when an external magnetic field is applied, yet they will
not show any magnetic interaction once the magnetic field is eliminated
[112]. The superparamagnetism is a characteristic strongly desired for
spinel ferrites to enhance water purification like the ease of their re­
covery from the reaction mixture by external magnetic field and possi­
bility of several times reuse. There are several factors such as method of
preparation, the cation distribution over the tetrahedral and octahedral
sites, crystalline size, sintering temperature, doping and dopant type can
affect the magnetic properties of ferrites. Houshiar et al. [113] studied
the effect of synthesis method on the size, structural, and magnetic
properties of CoFe2O4. They found that various methods of nanoparticle
A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Table 1 magnetization values increase with increasing the temperature as a

Advantages and disadvantages of synthesis methods of spinel ferrite result of the gradual increase in the crystallinity and particle size of the
nanoparticles. nanoparticles. Prasad et al. [115]. synthesized MFe2O4 (M = Zn, Ni, Cu,
Method/Process Advantages Disadvantages and Co) by auto-combustion route. Among all synthesized catalysts,
Solid state Economical, fast and easy to Spinel phase not always pure,
cobalt ferrites showed the highest saturation magnetization (41 emu/g),
implement. chemical inhomogeneity, whereas zinc ferrite displayed a low saturation magnetization value
nonuniformity of particle size (12.87 emu/g). The strong ferromagnetic nature of the cobalt ion is
and shape, formation of responsible for this high value. Hema et al. [116] fabricated
strongly bonded
MnxZn1− xFe2O4 (0.0 ≤ x ≤ 1.0) by a facile one-pot microwave com­
agglomerates, and high
annealing temperature. bustion method using urea as the fuel. The effect of Mn2+ doping on the
Co–precipitation Homogeneous mixing of Probability of impurity structural, morphological and magnetic properties was investigated. The
reacting materials, reduction formation, incomplete results showed that ZnFe2O4 have the lowest saturation magnetization
in the reaction temperature, precipitation, time (2.598 emu/g) and it increased with increasing Mn2+ dopant (from 0.2
and uniform sized nano consuming, little or no
particle formation. morphological control, and
to 1). For this reasons, these factors must be taken into consideration
non-homogeneous particle before prepared this materials and used in wastewater treatment as
size. catalyst or any fields. The preparation methods, particle size, shape,
Sol–Gel Low temperature synthesis, Low yield, evolution of large calcination temperature and the properties magnetic are given in
good chemical homogeneity, amounts of gasses, and
Table 2.
high product purity and contamination by
crystallinity, control in carbonaceous residues.
morphology, fine particle size 5. Application of SFs as catalysts in heterogeneous Fenton and
and narrow particle size photo-Fenton oxidation of different pollutants
distribution, simple
equipment and preparation
process, sintering at low
Spinel ferrites are more environmentally friendly, stable, reusable
temperature, and low cost and easy to separate from the reaction system compared to different
compared to conventional iron-based materials utilized as catalysts in heterogeneous Fenton and
ceramic process. photo-Fenton-like oxidation. The increasing trend of interest of these
Micro-emulsion Single phase, cost effective, Less yield, presence of
materials can be estimated from Fig. 9, in which the number of pub­
uniform crystalline structure, impurities, large amounts of
and control of particle size surfactant and/or lished research papers has been increased in these recent years. Among
and morphology. cosurfactant, generally different spinel ferrites reported in literature, magnetite Fe3O4, mag­
irritating at high nesium ferrite MgFe2O4, copper ferrite CuFe2O4, manganese ferrite
concentrations, and MnFe2O4, nickel ferrite NiFe2O4, zinc ferrite ZnFe2O4 and cobalt ferrite
temperature dependent.
CoFe2O4 are the most utilized in heterogeneous Fenton and photo-
Solvo(Hydro) Powder directly formed from High pressure, special reactor
thermal solution, control of particle required (autoclave), and the Fenton-like oxidation.
size, resulting powder is slurry formed is highly
highly reactive in nature, and corrosive in nature. 5.1. Magnetite Fe3O4
versatile method to prepare
various catalysts.
Template Good dispersion, uniform NR Magnetite is one of the most common natural occurring iron oxides.
method pore size, control of the It is a cubic inverse spinel ferrite material, which has attracted the
morphology, and simple attention of researchers due to its unique properties such as super­
operation. paramagnetism, relatively high activity, wide availability, low cost, low
Sono-chemical Facile control of reaction NR
conditions, good control of
toxicity, easy magnetic separation from the reaction medium and
particle size distribution, biocompatibility [121,122]. Fe3O4 nanoparticles are attractive hetero­
cost-effectiveness, high geneous Fenton-like catalysts for oxidative degradation of organic pol­
reaction rate, high purity. lutants with H2O2. Moreover, Fe3O4 comprises Fe(II) and Fe(III)
Electrochemical The possibility of controlling Produces poorly ordered
together, which according to Eq (1) and Eq (2) should have a positive
particle size in a range that is products, amorphous
difficult to achieve with other impurities, and effect on the catalytic activity. He et al. [123] reported the successful
synthesis techniques electrodeposition is only able degradation of catechol and 4-chlorocatechol catalyzed by nano-Fe3O4
(between 20 and 40 nm), and to perform on conducting within 3 h. Xu and Wang [124] reported the successful degradation of 2,
being an environmentally substrates. 4-dichloropheno by a Fenton-like reaction with Fe3O4 nanoparticles at
friendly process.
acidic medium. Furthermore, Zhang et al. [125] studied the oxidation of
*NR: Not reported. phenol and aniline by Fe3O4 nanoparticles. The results showed that both
phenol and aniline could be eliminated completely under optimized
synthesis can lead to different particle sizes and magnetic properties. Hc conditions and Fe3O4 was readily separated from solution by applying
and Ms are greatest in the combustion method (56.7 emu/g) and least in an external magnetic field. Wang et al. [126] used Fe3O4 nanoparticles
precipitation method (47.2 emu/g). Similarly, Kaur et al. [51]. prepared prepared by reverse co-precipitation method under the assistance of
MgFe2O4 by five methods, co-precipitation, sol-gel and combustion ultrasound irradiation in heterogeneous Fenton oxidation of Rhodamine
methods (Polyethylene glycol (PEG), urea and oxalyl dihydrazide (ODH) B. It was found that almost all the added Rhodamine B (0.02 mmol /L)
were used as fuel), keeping uniform calcination temperature and sin­ was completely removed within 60 min. Velichkova et al. [127] inves­
tering time. Differences in crystallinity, particle size and magnetic pa­ tigated the heterogeneous Fenton oxidation of paracetamol using three
rameters of Mg-ferrites by different methods were observed. Ghumare types of iron oxides as catalysts: nano- and submicro-structured
et al. [114]. studied the role of varying pH and calcination temperature magnetite and nano-structured maghemite. The influence of reaction
on the properties of CuFe2O4 prepared by sol–gel auto-combustion conditions such as temperature, iron amount, and hydrogen peroxide
method. The results showed that increasing pH value contributed to dosage were also investigated. The results showed that paracetamol
increase particle size. The magnetic properties are strongly influenced could be eliminated completely under optimized conditions after 5 h of
by sintering temperature. It can be observed that the saturation reaction time. Sun et al. [128] studied the oxidation of carbamazepine
and ibuprofen by heterogeneous Fenton-like oxidation using

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A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Fig. 8. Hysteresis loop of magnetic nanoparticles.

Table 2
Summary of the magnetic properties of the synthesized spinel ferrites nanoparticles.
Catalyst Method/Process Size (nm) Shape Calcination T( ◦ C) Ms (emu/g) Mr (emu/g) Mc (Oe) Ref

CoFe2O4 Combustion 69.5 – – 56.7 – 2002 [113]

coprecipitation 49.5 – – 55.8 – 850
precipitation 34.7 – – 47.2 – 233
MgFe2O4 Sol-gel 16.0 – 500 13.22 3.62 130.55 [51]
Co-precipitation 13.5 rectangular 500 1.95 – 2.59
Combustion (PEG) 16.0 Spherical 500 13.55 0.89 55.47
Combustion (urea) 8.0 Spherical 500 10.73 1.36 112.02
Combustion (oxalyl dihydrazide) 11.0 Spherical 500 13.25 3.45 66.05
NiFe2O4 Sol-gel (Citric acid) 12.91 – – 27.05 8 485 [117]
Sol-gel (PVA) 8.38 – – 24.49 9.75 489
Sol-gel (Urea) 3 – – 20.05 5.5 355
CuFe2O4 Sol–gel (Citric acid) 25.20 – 600 15.25 – – [114]
32.36 – 800 19.26 – –
34.39 – 1000 25.15 – –
ZnFe2O4 Sol–gel (Citric acid) 22 – – 12.87 3.37 352.12 [115]
NiFe2O4 23.2 – – 29.28 9.7 487.38
CuFe2O4 18.4 – – 24 9.21 497.72
CoFe2O4 27.2 – – 41.64 16 1597.1
CuFe2O4 Co-precipitation 15.4 particles 600 27.35 0 0 [118]
Hydrothermal 22.9 particles – 51.54 0 0
Sol-gel (Ethylene glycol) 33.1 Irregular blocks 800 33.24 17.15 473.35
Solid reaction 22.8 Particles 500 20.93 2.03 78.37
CoFe2O4 Plasma 40 – – 75.4 32.0 780 [119]
Combustion 20 – – 53.4 20.3 1170
Hydrothermal 10–12 – – 50.1 12.6 390
NiFe2O4 Plasma 40 – – 44.2 10.0 74
Combustion 10 – – 21.4 2.3 81
Hydrothermal 22 – – 39.0 2.6 23
ZnFe2O4 One-pot microwave combustion 37.57 Spherical – 2.598 0.014 7.472 [116]
Mn0.2Zn0.8Fe2O4 35.62 Spherical – 5.868 0.162 19.65
Mn0.4Zn0.6Fe2O4 32.35 Spherical – 23.06 1.134 23.72
Mn0.6Zn0.4Fe2O4 25.43 Spherical – 36.75 2.015 37.42
Mn0.8Zn0.2Fe2O4 26.85 Spherical – 48.09 8.473 53.93
MnFe2O4 27.91 Spherical – 60.99 11.48 64.78
CoMn0.2Fe1.8O4 Sol–gel (Citric acid)) 43 spherical 1000 74.3 20.8 623 [120]
CoMn0.4Fe1.6O4 41 spherical 1000 66.1 20.7 385
CoMn0.6Fe1.4O4 54 spherical 1000 58.1 14.1 220
CoMn0.8Fe1.2O4 55 spherical 1000 47.1 10.6 174
CoMnFeO4 46 spherical 1000 43.7 10.5 142

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A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

3. The preparation methods, process, applications, operating conditions

and Fenton catalytic activity of Fe3O4 are given in Table 3.

5.2. Magnesium ferrite (MgFe2O4)

Magnesium ferrite (MgFe2O4), is a soft magnetic material and be­

longs to the type partially inverse spinel, which already has attracted a
great deal of attention due to its good magnetic, electric properties,
excellent physical-chemical stability, and mechanical strong point [13].
A diverse and broad range of applications for this material is known
which include catalysis, transformer cores, microwave devices,
high-density recording media, humidity and gas sensors [133,134].
However, as far as we know, most studies on degradation properties of
magnesium ferrite are focused on its photocatalytic [135] or photo­
electrochemical [136] performance. Few reports have been published
on the application of magnesium ferrite as heterogeneous Fenton cata­
lytic agents. Ivanets et al. [59] synthesized MgFe2O4 nanoparticles by
glycine-nitrate method and used it as Fenton-like catalysts for methylene
blue degradation in aqueous solutions under visible light. It was deter­
Fig. 9. Evolution of the number of scientific papers devoted to the applications
mined that dye mineralization rate achieved 98% within 30 min under
of spinel ferrite in heterogeneous Fenton processes. Source: Web of Science;
visible light. Zhang et al. [90] prepared MgFe2O4 nanorods by template
Topic: “ferrite” and “Fenton” and “Catalytic Wet Peroxide Oxidation”; Search­
ing time: 15 June 2021.
method, for the degradation of Congo red dye by Fenton oxidation. They
found that the degradation of the dye with MgFe2O4 nanorods is better
than that of nanoparticles. The degradation rate of Congo red attained
nano-magnetite. It was demonstrated that the nano-Fe3O4 catalyzed
95% after 2 h. Also, after five cycles, the catalytic activity remained
heterogeneous Fenton-like reaction was successful in degrading carba­
almost invariable. Furthermore, Das et al. [137] fabricated MgFe2O4
mazepine and ibuprofen in aqueous suspensions at neutral pH. The in­
nanoparticles by solid-state reaction method and was used as a catalyst
fluence of important factors pH, H2O2 and catalyst doses determined by
for the degradation of malachite green dye. The catalyst showed 100%
experimental design methodology provides a range of optimum condi­
degradation of the dye in 50 s in the presence of H2O2. Diao et al. [138]
tions that will allow the system to be tested under realistic working
synthesized magnesium ferrite from saprolite laterite for the degrada­
conditions that take into account economic practicalities. More recently,
tion of Rhodamine B dye by Fenton and photo-Fenton oxidation. They
Wan et al. [129] fabricated Fe3O4 nanoparticles by a simple oxida­
found that the doped MgFe2O4 exhibited degradation efficiency up to
tion–precipitation method and used as Fenton-like catalysts for rhoda­
96.8% under visible light illumination within 3 h. Also, they found that
mine B degradation. The material exhibited spherical morphology with
the catalyst is more competitive compared to other catalysts prepared
different particle sizes (30, 70, 250, and 600 nm). The results showed
from pure chemical agents. Similarly, Han et al. [139] found that
that catalytic activity increased with the reduced particle size (30 nm >
MgFe2O4 presented favorable catalytic activity for the degradation of
70 nm > 250 nm > 600 nm). Besides, Jiang et al. [130] studied the
Rhodamine B, 97.8% degradation efficiency of 10 mg/L dye concen­
degradation of dinitrotoluene by Nano-Fe3O4/H2O2. The results showed
tration within 300 min. The preparation method, process, applications,
that the catalytic reaction system within the pH value range of 1 to 9
operating conditions and Fenton catalytic activity of MgFe2O4 are given
could effectively degrade di-nitrotoluene, and the optimal pH value was
in Table 4.

Table 3
Summary of the application of magnetite ferrite in heterogeneous Fenton-like oxidation of pollutants.
Preparation method Molecule Catalytic activity Reaction conditions Ref.
Catalyst Pollutant H2O2 pH T(
(g/L) (mg/L) (mM) ◦
C)

Coprecipitation 4‑chloro-catechol Complete oxidization within 1 144.56 50 6.5 25 [123]

3 h.
Coprecipitation 2,4-dichlorophenol Complete decomposition and 1.0 100 12 3 30 [124]
51% of TOC removal after 3 h.
Coprecipitation Phenol and aniline. Complete removal after 6 h. 5 93.13–94.11 1200 Acidic and 35 [125]
neutral
medium
Ultrasonic-assisted reverse co- Rhodamine B 90% conversion in 1 h. 0.6 9.58 40 5.4 40 [126]
precipitation
supplied by Sigma-Aldrich paracetamol Complete degradation after 5 6 100 153 2.7 60 [127]
h.
obtained from Nanostructured & Carbamazepine and Degradation efficiencies 1.84 15 600 Neutral pH 23 [128]
Amorphous Materials Inc. (Houston, ibuprofen between 83 and 87% in 12 h.
Texas)
Oxidation–precipitation Rhodamine B Around 96.3% conversion in 1 40 50 3 25 [129]
5 h.
Coprecipitation di-nitrotoluene 97.6% degradation in 2 h. 1.0 100 7.056 3 25 [130]
obtained from Nanostructured & p-Nitrophenol 90% degraded after 10 h. 1.5 25–45 620 7.0 22 [131]
Amorphous Materials Inc. (Texas,
USA).
Co-precipitation Phenol 60% conversion in 24 h. 3 25 147.05 Neutral pH 22 [132]

Note: Abbreviation: not reported “NR”.

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A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Table 4
Summary of the application of magnesium ferrite in heterogeneous Fenton-like and photo-Fenton-like oxidation of pollutants.
Preparation method Process Molecule Catalytic activity Reaction conditions Ref.
Catalyst Pollutant H2O2 pH T ( ◦ C) Light
(g/L) (mg/L) (mM)

Glycine-nitrate method photo- Methylene Mineralization rate 0.5 10 20 8 20 visible [59]

Fenton- blue achieved 98% in 30 min. light
like
Template method photo- Congo red 95% degraded within 2 h. 0.4 20 2.20 Not 80 150 W [90]
Fenton- adjusted Xenon arc
like lamp
Solid-state reaction Fenton- Malachite The degradation rate of 0.571 10 0.294 7 Ambient – [137]
method. like green MG attained 100% after
50 s.
Hydrothermal method photo- Rhodamine 96.8% for photo-Fenton- 1 10 88.2 6.82 NR 500 W [[138]
from saprolite laterite Fenton- B like degradation of RhB in xenon
ore like 3 h. lamp
Hydrothermal- Fenton- Rhodamine 97.8% degradation 0.625 10 88.2 6.44 45 – [139]
calcination method like B efficiency within 5 h.
from saprolite laterite

NR: not reported.

5.3. Copper ferrite (CuFe2O4)
Copper ferrite is one of the important spinel ferrite with paramount
advantages over other type of magnetic materials due to its unmatched
flexibility in magnetic and mechanical parameters, thermal stability,
chemical stability, high photochemical stability, semiconducting,
excellent magnetic properties and light response, electrical properties,
and low cost [140,141]. Copper ferrite can exist in two crystallographic
forms, as cubic or tetragonally distorted structures, depending on the
preparation method and calcination temperature and according to the
concentration of distorting Jahn-Teller Cu2+ ions in B sites of the spinel
structure [142]. The cubic structure is stable below 300 ◦ C and the
tetragonal is stable over 400 ◦ C [143,144]. The phase transformation is
irreversible, because of the greater thermodynamic stability of the
tetragonally distorted versus cubic spinel [145].
Currently, spinel copper ferrites CuFe2O4 have received intensive
attention in heterogeneous Fenton oxidation due to its different prop­
erties. Feng et al. [60] evaluated the activity of CuFe2O4 spinel nano­
particles in heterogeneous Fenton oxidation of sulfanilamide. The
influence of reaction conditions such as oxidant dosage, catalyst loading
was investigated. They highlighted that under the optimal conditions
near-total degradation of sulfanilamide was achieved. The oxidant
dosage and catalyst loading influenced the degradation of sulfanilamide
and the stoichiometric efficiency values of H2O2. Cheng et al. [146]
studied the degradation of glycerol aqueous solution by
photocatalytic-Fenton technique. Results showed that the degradation
of glycerol improved substantially to record nearly 40.0% degradation
at a catalyst loading of 5 g/L. This has demonstrated that the copper
ferrite under the visible light was capable of generating additional hy­
droxyl radicals to attack the glycerol molecule. Furthermore,
Tehrani-Bagha et al. [147] reported the successful degradation of
reactive red 120 catalyzed by copper ferrite nanoparticles at pH 3 and
75 ◦ C. Dang et al. [61] evaluated the activity of CuFe2O4 in heteroge­
neous Fenton oxidation of methylene blue. The dye was almost
completely degraded after 3 h and its activity was unchanged after 5
time reuse. Moreover, López-Ramón et al. [148] studied the effect of the
calcination temperature of CuFe2O4 on its crystalline phase formation
and transformation, catalytic activity, metal ion leaching and reutili­
zation in heterogeneous Fenton oxidation of gallic acid. The results
demonstrated that copper ferrite catalyst shows good activity, the per­
centage of degradation and TOC removal at 15 min of reaction were 98
and 95%, respectively. Guo et al. [149] applied CuFe2O4 as catalyst in
the heterogeneous photo-Fenton-like oxidation of methylene blue. They
found that the introduction of tartaric acid enhanced methylene blue
decolorization rate from 52.0% to 92.1% within 80 min. In another
research, Gao et al. [150] and Wang et al. [151] fabricated CuFe2O4
using KIT-6 as template through the hard template strategy, and used as
heterogeneous Fenton-like catalyst for removing of sulfonamide anti­
biotics and imidacloprid respectively. They found that the catalytic ac­
tivity of the catalysts with ordered mesoporous structure is superior to
non-mesoporous structure, suggesting the high efficiency of catalysts,
related with their high surface area and large pore size. Moreno-Castilla
et al. [79] prepared copper ferrite nanosphere by solvothermal method
and tested as Fenton catalysts in the mineralization of phenol, p-nitro­
phenol and p-aminophenol. They found that the degradation of all
phenols was practically complete with 95% total organic carbon (TOC)
removal. The catalytic activity of phenolic compounds increased in the
order phenol < p-nitrophenol < p-aminophenol and decreased when the
calcination temperature was raised. Yu et al. [152] fabricated
nanoscale-confined precursor of CuFe2O4 using a facile co-precipitation
method with the confinement of hyperbranched polyamide and used as
Fenton catalysts in the mineralization of reactive red 2. The results
showed that around 91.3% of the dye was removed after 60 min without
pH adjustment. Flores et al. [153] also established that spinel copper
ferrite nanoparticles an eminently performance in heterogeneous
photo-Fenton discoloration/degradation of Rhodamine B. The prepara­
tion methods, process, applications, operating conditions and Fenton
catalytic activity of CuFe2O4 are given in Table 5.
5.4. Manganese ferrite (MnFe2O4)
MnFe2O4, a well-known soft magnetic material, has attracted the
attention of researchers due to its mesmerizing magnetic, electromag­
netic properties, low cost, high surface area, good chemical stability,
mechanical hardness, catalytic properties and environmentally friendly
[154,155].Furthermore MnFe2O4 belongs to a group of soft magnetic
materials which are used in different areas such as adsorbents, recording
media devices, drug delivery, hyperthermia, ferrofluid and biosensors.
Khan et al. [50] synthesized MnFe2O4 by simple co-precipitation method
and successfully used as an efficient heterogeneous photo-Fenton for the
photocatalytic degradation of crystal violet. The degradation rate was
90% within 60 min. Wang et al. [156] fabricated MnFe2O4 using sol-gel
method. The MnFe2O4/H2O2 system was able to remove 90.6% of nor­
floxacin at neutral pH, and the spent material can be reused in multiple
cycles of operations. Moreover, MnxFe3− xO4 were synthesized by a
simple one-step solvothermal route by Li et al. [84] and tested in cata­
lyzing the degradation of methylene blue. It was identified that the
chemical composition had a significant influence on the physicochem­
ical characteristics of MnxFe3− xO4 samples. Also, they reported that
Mn1.07Fe1.93O4, had a much higher activity than other Fe-based or

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A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Table 5
Summary of the application of copper ferrite in heterogeneous Fenton-like and photo-Fenton-like oxidation.
Preparation method Process Molecule Catalytic activity Reaction conditions Ref.
Catalyst Pollutant H2O2 pH T ( ◦ C) Light
(g/L) (mg/L) (mM)

Sol-gel combustion Fenton- Sulfanilamide Near-total degradation 0.5 0.55 15 6.5 25 – [60]
(citrate-method) like was achieved in 3 h.
Sol-gel (Pechini method) Fenton- Methylene Near-total degradation 2.0 9.5955 352.8 6.5 40 – [61]
like blue within 3 h.
Solvothermal method Fenton- 3 phenolic Complete degradation of 0.1 10.07–14.88 1.40–1.50 3 35 – [79]
like compounds all phenols with 95% TOC
removal.
Sol-gel (citrate method) Photo- Glycerol About 40% degradation 5 6299.21 819.5 NR Ambient 250 W [146]
Fenton- was achieved after 4 h. xenon lamp
like
Polymeric precursor Fenton- Reactive Red ~95% removal after 50 0.02 50 10 3 75 – [147]
method like 120 min.
Sol-gel combustion Fenton- Gallic acid 98% removal after 15 min 0.05 20.41 2.64 4.3 35 – [148]
(citrate-method) like of reaction.
Sol-gel combustion EG Photo- Methylene 92.1% degradation 0.2 50 20 5 25 UV lamp [149]
Fenton- blue within 80 min (in the (365–450
like presence of 1 mM of nm)
tartaric acid
Template method Photo- sulfonamide Complete transformation 0.2 10 10 6.73 – 300 W [150]
Fenton- within 2 h. xenon lamp
like
Template method Fenton- Imidacloprid 100% removal efficiency 0.3 10 40 3 30 – [151]
like after 5 h.
Coprecipitation with the Fenton- Reactive red 2 Around 91.3% of removal 0.217 100 852.17 ~7.9 50 – [152]
confinement of like after 60 min.
hyperbranched
polyamide
Wet-chemical synthetic Photo- Rhodamine B 95% discoloration in 10 0.4 9.5804 83 6.2 22 UV (254 [153]
Fenton- min, and 97% nm)
like degradation in 200 min.

NR: not reported.

Table 6
Summary of the application of manganese ferrite in heterogeneous Fenton-like and photo-Fenton-like oxidation.
Preparation Process Application Catalytic activity Reaction conditions Ref
method Catalyst Pollutant H2O2 pH T( Light
(g/L) (mg/L) (mM) ◦
C)

Co-precipitation photo- Crystal violet 90% degradation rate after 0.1 10 88.2 7.5 NR 50 W Mercury [50]
Fenton-like 60 min. vapor lamp
Auto combustion photo- Methylene complete removal after 80 NR 10 10 NR NR Sunlight [66]
Fenton-like blue min.
Solvothermal Fenton-like Methylene 98.2% degradation rate 0.5 400 1323 NR 30 – [84]
blue after 360 min.
Sol gel- Fenton-like Norfloxacin. 90.6% removal after 180 0.6 10 200 6.6 NR – [156]
hydrothermal min.

NR: not reported.

Mn-based heterogeneous catalysts reported in the literatures. The
preparation methods, process, applications, operating conditions and
Fenton catalytic activity of MnFe2O4 are given in Table 6.
5.5. Nickel ferrite (NiFe2O4)
Nickel ferrite is a soft magnetic material with an inverse spinel
structure, is the matter of research for several decades due to their
interesting propriety including magnetic, electric, low conductivity,
abundance in nature, stable thermal ability, high electrochemical sta­
bility, high resistivity and thermal durability and catalytic behavior
[157,158]. NiFe2O4-based materials have found applications in cata­
lysts, magnetic adsorbents, MRI contrast agents, ferro-fluids, high fre­
quency devices, magnetic refrigerators, microwave devices, electronic
devices, computer memories, etc. Vinosha et al. [159] synthesized
NiFe2O4 by low-temperature coprecipitation technique and was used in
photo-Fenton degradation of methylene blue. The results show that in
the absence of light methylene blue+H2O2+NiFe2O4 showed ~30%
degradation, but the degradation improved to ~99% in the incidence of
light. Additionally, the results indicated that the catalyst could be reused
up to five cycles without any momentous loss which triggers its appli­
cations for photo-Fenton activity in wastewater treatment and in
pollution control. Costa et al. [160] have performed a comparative
studies on Fe3-xMxO4 (M = Fe, Co, Mn, Ni) as heterogeneous Fenton
catalysts. They compared the effects of Co, Mn, and Ni substitution on
H2O2 decomposition. They concluded that incorporation of M2+ species
into the magnetite structure resulted in a remarkably increased reaction
activity. On the other hand, the presence of nickel inhibited the reaction
and as the Ni concentration in the magnetite increased the reaction rate
decreased. From this point, Liu et al. [78] have employed NiFe2O4
synthesized by hydrothermal method as a magnetic catalyst for the
photo-Fenton degradation of rhodamine B in the presence of oxalic acid.
They reported that similar to H2O2, oxalic acid in the Fenton system can
split the bonds of organic molecules and decolorize dye molecules. The
results show that the 1.0 mM oxalic acid reaches an optimal degradation
rate at pH 3.0 (98.7% decolorization ratio is reached after 60 min). Guo

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A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

et al. [82] have fabricated NiFe2O4 hallow nanospheres by solvothernal
process and were employed in photo-Fenton degradation of methylene
blue in the presence of hydrogen peroxide, oxalic acid and visible light.
98.5% degradation in 50 min was achieved. Whereas, when the light
source was off, the decolorization rate was only 18.8% under similar
conditions which indicated that visible light irradiation played an
important role in this system. In the absence of hydrogen peroxide and
oxalic acid the decolorization rate was 52.3% and 13.4% respectively.
This result shows that oxalic acid is significant to the photo-Fenton
process. The preparation methods, process, applications, operating
conditions and Fenton catalytic activity of NiFe2O4 are given in Table 7.
5.6. Zinc ferrite (ZnFe2O4)
Zinc ferrite ZnFe2O4 with a normal spinel, has long been the subject
of studying because of its contrasting magnetic properties as compared
with other spinel ferrites and the unique electric, magnetic, catalytic
properties, chemical and thermal stability [161,162]. Zinc ferrite is
spinel oxide that has a cubic structure and great potential in various
technology applications such as gas sensor, hyperthermia, magnetic and
superparamagnetic materials adsorbents, materials with optical and
dielectric properties, antibacterial agent, contrast agents, catalysts and
photocatalysts etc. Cai et al. [163] have fabricated ZnFe2O4 catalyst by
two-step via novel reduction oxidation route, and used as a magnetic
catalyst for the photo-Fenton degradation of orange II. The result shows
that the catalyst exhibited good activity and stability under visible
irradiation. The decolorization rate was still over 94% after five reuse
cycles and extremely low leaching of zinc and iron were observed.
Mahmoodi [164] fabricated ZnFe2O4 as photo-Fenton catalyst to
remove reactive dyes (reactive red 198 and reactive red 120). The re­
sults indicated that ZnFe2O4 could be used as a magnetic catalyst to
degrade dyes in wastewater. Su et al. [77] reported the synthesis of
mesoporous zinc ferrite using a hydrothermal process and was employed
in photo-Fenton degradation of acid orange II. The degradation in the
H2O2-ZnFe2O4-visible light system was almost complete within 2 h.
Additionally, Anchieta et al. [165] prepared zinc ferrite ZnFe2O4 oxide
by microwave-solvothermal technique and applied as heterogeneous
photo-Fenton catalyst for the removal of Reactive red 141. The reaction
results showed that the ZnFe2O4 oxide has good photocatalytic activity,
nearly 100% of decolorization at 40 min and 60% of mineralization at
240 min. The preparation methods, process, applications, operating
conditions and Fenton catalytic activity of ZnFe2O4 are given in Table 8.
5.7. Cobalt ferrite (CoFe2O4)
In the family of spinel ferrites, cobalt ferrite is a unique ferrite having
inverse spinel structure and is a well-known hard magnetic material,
possessing strong magneto-crystalline anisotropy, high corecivity,
moderate saturation magnetization, large magnetostrictive coefficient,
wear resistance, electrical insulation, remarkable chemical stability,
mechanical hardness, high electrical resistance with low eddy current
losses [166–168]. These properties make it a promising material for high
density storage devices, sensor, semiconductor photocatalysts, ferro­
fluid, hyperthermia, magnetic resonance imaging (MRI), magnetic sep­
aration, drug delivery, biosensing, magnetofection, cancer treatment,
audio and videotapes, photo-detectors, magnetic optical behavior,
electrical and antibacterial.
Vinosha and Das [49] fabricated cobalt ferrite nanoparticles by
co-precipitation route and were employed in photo-Fenton degradation
of methylene blue dye. The degradation rate was nearly 99.3% in 75
min. Also, Kalam et al. [83] prepared cobalt ferrite nanoparticles using
modified solvothermal method for the degradation of methylene blue in
the presence of H2O2 and visible light. The results showed 80% degra­
dation of methylene blue within 140 min. Rad et al. [169] compared the
degradation of phenol, during photo-Fenton-like process using cobalt
ferrite synthesized by hydrothermal and microwave methods. The mi­
crowave synthesized cobalt nanoferrite exhibited the better activity for
phenol degradation compared with cobalt nanoferrite obtained by hy­
drothermal process. de Souza et al. [170] fabricated cobalt ferrite by a
novel unconventional coprecipitation procedure (UCP) followed by a
simple and fast microwave-assisted hydrothermal (MAH) treatment and
were employed in photo-Fenton degradation of lignin. 25% of the lignin
was degraded over the CoFe2O4/MAH ferrite after 4 h reaction time.
Furthermore, Rad et al. [171] synthesized cobalt ferrite using micro­
wave heating method and compared adsorption and photo-Fenton pro­
cesses for phenol and paracetamol removing from aqueous solutions.
The results showed that photo-Fenton process was found to be as an
alternative method for the treatment of phenol and paracetamol from
wastes at higher initial concentrations. The preparation methods, pro­
cess, applications, operating conditions and Fenton catalytic activity of
CoFe2O4 are given in Table 9.
5.8. Comparison
Sharma et al. [172] systematically studied spinel ferrites MFe2O4 (M
= Co, Cu, Ni and Zn) in the presence of hydrogen peroxide and potas­
sium peroxymonosulfate in photo-Fenton-like oxidation process, for
deterioration of different phenolic derivatives. They reported that
among all four synthesized catalysts CuFe2O4 and CoFe2O4 possessed
excellent ability to activate hydrogen peroxide and peroxymonosulfate,
respectively. The photo-Fenton activity of ferrites was extended to the
degradation of different nitro- and chloro‑analogs of phenol (2-nitro­
phenol, 3-nitrophenol, 4- nitrophenol, 2,4-dinitrophenol, 2,4,6-trini­
trophenol, 2-chlorophenol, 3-chlorophenol, 4-chlorophenol, 2,4-
dichlorophenol) with only two ferrites (CuFe2O4 and CoFe2O4). Also,
Sharma et al. [173] applied the same catalysts MFe2O4 (M = Co, Cu, Ni

Table 7
Summary of the application of nickel ferrite in heterogeneous Fenton like and photo-Fenton like oxidation.
Preparation Process Application Catalytic activity Reaction conditions Ref
method Catalyst Pollutant H2O2 Oxalic pH T( Light
(g/L) (mg/L) (mM) acid ◦
C)
(mM)

Hydro-thermal photo- Rhodamine 98.7% 2 10 – 1 3.0 25 300 W UV–Vis [78]

Fenton- B decolorization after lamp
Like 60 min.
Solvothermal photo- Methylene 98.5% degradation 0.2 30 5 0.666 Not NR 300 W UV- [82]
Fenton- blue in 50 min. adjusted curing lamp (λ
Like > 400 nm)
Fenton- 18.8% degradation 0.2 30 5 0.666 Not NR –
Like in 50 min. adjusted
low-temperature photo- Methylene 99% degradation in 1 10 352.8 – NR NR 125 W mercury [159]
coprecipitation Fenton- blue. 90 min. lamp
Like

NR: not reported.

12
A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

Table 8
Summary of the application of zinc ferrite in heterogeneous photo-Fenton-like oxidation.
Preparation method Application Catalytic activity Reaction conditions Ref.
Catalyst Pollutant H2O2 pH T( Light
(g/L) (mg/ L) (mM) ◦
C)

Hydrothermal Orange II Complete degradation within 2 h. 0.5 100 12 6 NR 150 W Xenon arc [77]
process lamp
Reduction- Orange II Decolorization efficiency was 94.9% 0.5 100 5 6 20 150 W Xenon [163]
oxidation method after 60 min reaction. lamp
– Reactive red 198 and ~100% decolorization in 60 min. 0.25 100 1.2 NR 25 UV-C lamp [164]
Reactive red 120 (200–280 nm, 9
W)
Microwave- Reactive red 141 ~100% of decolorization at 40 min 0.5 65 20 2 NR 85 W, (λ~400 [165]
solvothermal and 60% of mineralization at 240 min. nm),

NR: not reported.

Table 9
Summary of the application of cobalt ferrite in heterogeneous photo-Fenton-like oxidation.
Preparation method Application Catalytic activity Reaction conditions Ref
Catalyst Pollutant H2O2 pH T( Light
(g/L) (mg/L) (mM) ◦
C)

Co-precipitation Methylene blue ~99.3% degradation of in 1 20 264.6 NR NR 125 W mercury [49]

75 min Lamp
Modified Solvothermal Methylene blue 80% degradation within 0.01 10 5.0 NR NR solar light simulator [83]
140 min
Hydrothermal and microwave Phenol Complete degradation 0.3 100 30 3 35 4 UV lamps (15 W, [169]
after 2 h. λmax = 365 nm)
Co-precipitation) followed by Lignin 25% degradation over 0.5 100 28.73 3 27 4 low-pressure [170]
microwave-assisted hydrothermal CoFe2O4/MAH after 4 h mercury lamps (15
(MAH) W)
Microwave heating Phenol and 99% removal after 1h 0.2 20 50 3 45 4 UV lamps (15 W, [171]
paracetamol λmax = 365 nm)

NR: not reported.

Table 10
Summary of literature works reported comparative studies of the catalytic activity of metal ferrites in heterogeneous Fenton oxidation.
Catalyst Preparation Process Application Catalytic activity Reaction conditions Ref.
method Catalyst Pollutant H2O2 pH T( Light
(g/L) (mg/L) (mM) ◦
C)

MFe2O4 (M = Sol-gel photo- p- The rate of the reaction 0.5 29.21 8.8 2.5 NR Xe-lamp [172]
Co, Cu, Ni Fenton- nitrophenol decreased in the order (150 W,
and Zn) like CuFe2O4 > ZnFe2O4 > Philips)
NiFe2O4 > CoFe2O4 and
CoFe2O4 > CuFe2O4 >
NiFe2O4 > ZnFe2O4 while
using HP and PMS as
oxidants respectively
0.5 29.21 2.2 Not NR
mM adjusted
(PMS).
MFe2O4 Sol-gel Fenton- Remazol In photo-Fenton process, the 0.5 50 8 2.5 NR 150 W [173]
(M=Cu, Zn, like and Black 5 reactivity decreases in the Xe-lamp
Ni and Co) photo- order CuFe2O4 > ZnFe2O4 >
Fenton- NiFe2O4 > CoFe2O4. In
like Fenton process the reactivity
decreases in the order
CuFe2O4 ~ CoFe2O4 >
NiFe2O4 > ZnFe2O4
CuFe2O4, – Fenton- Gallic acid CuFe2O4 > Fe3O4 > FeTiO3 0.05 20.41 2.64 4.3 NR – [174]
Fe3O4, and like
FeTiO3)
MFe2O4 (M = Sol-gel Fenton- Phenol CuFe2O4 > MgFe2O4 > 0.3 g/L 200 500 Not 25 – [176]
Cu, Mg, Zn like ZnFe2O4 adjusted
Fe3− xMxO4 Precipitation- photo- Tetrabromo- The incorporation of the 0.5 20 10 6.5 25 6 W UV- [177]
(M = Fe, Ti, oxidation Fenton- bisphenol A cations improved the UV/ light tube
Cr, Mn, Co like Fenton catalytic activity of (λ = 365
and Ni) magnetite in the following nm)
order: Co < Mn < Ti ≈ Ni <
Cr

NR: not reported.

13
A. SOUFI et al. Applied Surface Science Advances 6 (2021) 100145

and Zn) as heterogeneous Fenton and photo-Fenton catalyst for the Table 11
degradation of Remazol Black 5. Among all the four ferrites CuFe2O4 Spinel ferrites used in wastewater treatment and their reuse performance.
was found to be best. Furthermore, Fontecha-Camara et al. [174] Catalysts Pollutant Number of Activity after Ref.
applied three commercial mixed iron oxides: copper ferrite (CuFe2O4), cycles reuses
magnetite (Fe3O4), and ilmenite (FeTiO3) as Fenton catalysts for the CuFe2O4 Reactive Red 120 6 No significant [147]
degradation and mineralization of gallic acid. The results illustrate that reactivity loss.
gallic acid was completely mineralized with the three catalysts in the CoFe2O4 Methylene blue 5 No significant [49]
following order of catalytic activity: CuFe2O4 > Fe3O4 > FeTiO3. Roo­ reactivity loss.
MFe2O4 (M=Co, different 4 No significant [172]
nasi et al. [175] compared a number of synthetic M-ferrite (where M = Cu, Ni and Zn). phenolic reactivity loss.
Zn, Mn, Fe and Cu) as the heterogeneous Fenton-like catalysts for effi­ derivatives
ciency against phenol removal in the presence of hydrogen peroxide. Co1-xZnxFe2O4 rhodamine B 5 No significant [178]
Among the studied catalysts, CuFe2O4 had higher catalytic activity for ((0 ≤ x ≤ 0.5) reactivity loss.
MFe2O4 (M=Cu, Remazol Black 5 4 No significant [173]
phenol removal at neutral pH. Hamdan et al. [176] prepared CuFe2O4
Zn, Ni and Co) reactivity loss.
nanoparticles by sol-gel auto combustion and co-precipitation methods MnFe2O4 norfloxacin 5 No significant [156]
and were employed for the degradation of phenol. They found that reactivity loss.
CuFe2O4 prepared by sol-gel route showed higher porosity, purity, CuFe2O4 Methylene Blue 5 No significant [61]
crystallinity and catalytic activity compared to the CuFe2O4 catalysts reactivity loss.
MgFe2O4 Congo Red 5 No significant [90]
obtained by the co-precipitation method. Also, they proved that spinel reactivity loss.
copper ferrites catalyst showed an eminently performance compared to NiFe2O4 rhodamine B 7 No significant [78]
TiO2, MgFe2O4 and ZnFe2O4, with the following order: CuFe2O4 > TiO2 reactivity loss.
> MgFe2O4 > ZnFe2O4. The preparation methods, process, applications,
operating conditions and Fenton catalytic activity of different ferrites
eminently performance and this is due to the synergic effects between Fe
are given in Table 10.
and Cu ions which can also the main active sites for HO• radical gen­
eration. Also, the pH of the solution, the concentration of ferrous ions,
6. Recovery and reuse
the concentration of hydrogen peroxide, the initial concentration of the
element to deteriorate, temperature and the power of the radiation
The regeneration and reuse of spinel ferrites after being used as
source are the main operating conditions that can affect the catalytic
catalysts with the same degradation efficiency is one of the key factors
activity of spinel ferrites. The optimal pH is often between 3 and 7 and
that make the process attractive in wastewater treatment. This reduces
the generation of OH radicals was maximum at pH0 = 3.0. The degra­
the cost of operation and has less impact on environment. Also, the
dation rate of organic compounds increases with an increase in initial
separation of the catalysts using an external magnetic field is superior to
H2O2 concentration until an optimum value is reached, after which it
the commonly used filtration and centrifugation process, since it is
decreases mainly due to scavenging of HO• by excess H2O2. The reaction
simple, selective and rapid. Based on this literature review, after each
temperature is another important process parameter, but rarely
reaction, the catalysts were simply washed with alcohols (ethanol,
addressed in the literature dealing with the use of spinel ferrite in the
methanol) or bases (NaOH, NaHCO3) or low concentrated acid (HCl,
Fenton process. It was observed that an increasing in the temperature
HNO3, H3PO4) or distillated water to remove any contamination after
leads to a faster generation of hydroxyl radicals by the Fenton reaction.
that they were dried in an oven at (80–100 ◦ C) and were used for another
Moreover, the degradation rate usually decreases when increasing the
oxidation cycle. Table 11 demonstrates the stability and reusability of
initial concentration of the pollutant due to an insufficient number of
different spinel ferrites nanoparticles; they had no significant reactivity
hydroxyl radicals. The type of the lamp used and its power may affect
loss even after several cycles. Therefore it was deduced that this mate­
significantly the performance in the photo-Fenton degradation; an in­
rials possesses high reactivity, good stability and ability to be magneti­
crease in the power of the radiation produces an increase in the catalytic
cally separated and used as sustainable and green catalysts in
activity. The catalytic activity of spinel ferrites is crucially related to
heterogeneous Fenton and the photo-Fenton-Like processes.
several parameters. Also, the higher specific surface area would help to
improve the catalytic properties of these materials, the higher surface
7. Conclusion
energy and the stronger magnetic of spinel ferrites often result in the
agglomeration of nanoparticles in some case. Because of this, the
The application of spinel ferrite nanoparticles as heterogeneous
modified structure of spinel ferrites deserves to be explored.
Fenton catalysts represents promising alternative compared to conven­
tional catalysts used in classical Fenton oxidation. Spinel ferrites have a
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