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Physical and photo-electrochemical properties of MgFe2O4 prepared by sol

gel route: application to the photodegradation of methylene blue

Article  in  Journal of Materials Science Materials in Electronics · February 2019

DOI: 10.1007/s10854-019-00830-2

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Journal of Materials Science: Materials in Electronics
https://doi.org/10.1007/s10854-019-00830-2

Physical and photo-electrochemical properties of ­MgFe2O4 prepared

by sol gel route: application to the photodegradation of methylene
blue
Z. Hammache1 · A. Soukeur1 · S. Omeiri2 · B. Bellal2 · M. Trari2

Received: 27 October 2018 / Accepted: 28 January 2019

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Abstract
The spinel M­ gFe2O4 synthesized by sol gel method, was characterized by physical and electrochemical methods. The thermal
analysis (TG) gives an optimal synthesis temperature −
of 650 °C where the X-ray diffraction pattern exhibits a single phase
crystallizing in a cubic symmetry (Space Group: Fd3 m) with spherical crystallites (~ 0.45 µm). The morphology observed
through the SEM image shows elliptical and spherical grains of ~ 0.8 µm. The spinel possesses a direct optical transition
(2.16 eV) due to electrons transfer F­ e3+: d−d transition, coming from the crystal field splitting in agreement with the red color.
The low electrons mobility is assigned to a narrow conduction band of ­Fe3+: 3d parentage with activation energy (0.14 eV)
in conformity with a conduction mechanism by small polaron hopping. The semi-logarithmic plot confirms the chemical
stability of oxide. Unlike other spinels, the capacitance plot exhibits n type conduction confirmed by chrono-amperometry
with a flat band potential (­ Efb) of 0.27 V. The electrochemical impedance spectroscopy displays a semi-circle attributed
to the bulk behavior. As application, the photodegradation of methylene blue (10 mg ­L− 1) was successfully on the spinel
suspension; 87% are eliminated after 2 h of exposure to sunlight irradiation.

1 Introduction degradation [11], water splitting and C ­ O2 conversion into

hydrocarbon fuels [12].
The spinel ­MgFe2O4 is formed from abundant elements (Mg, The spinel ferrite was synthesized by different methods
Fe, O) in the terrestrial crust, non-hazardous to the envi- the like sol gel [13], pulse laser deposition [14, 15] and
ronment. It possesses interesting photo catalytic properties hydrothermal, where the authors have used the hetero-junc-
and because to its red color, the oxide absorbs in the vis- tion ­Ag3PO4/MnFe2O4 for the degradation of methylene blue
ible region and is attractive for the solar energy conversion. (MB) and Rhodamine B under solar-light [16]. The spinels
­MgFe2O4 crystallizes in a cubic system and has various tech- were prepared by spray coating with enhanced cristallinity
nological applications such as anode material for lithium-ion and suppression of the charge carrier recombination [17].
batteries [1], catalytic activity [2, 3], gas sensor [4] electri- To increase the photo catalytic efficiency and to enhance
cal and magnetic behaviors [5], it has also been applied as the photocatalytic performance, a pre-polymerization was
adsorbent for ­Co2+ [6] and more recently in photocatalysis used, leading to an increased specific surface area and in
[7, 8]. The light-induced bleaching of methyl blue [9], in this way the active sites [18]. We have selected the sol gel
thin film showed the best photocurrent responses [10]. The route which gives small crystallites whose size approaches
photocatalysis over spinels has also been applied for the dyes the diffusion length of the minority carriers. The knowl-
edge of physical and electrochemical parameters permits to
* S. Omeiri draw the energy band diagram of the junction M ­ gFe2O4/
[email protected] electrolyte and to predict the mechanism of MB photo deg-
radation. MB is more and more used in the textile industry,
1
Laboratory of Hydrometallurgy and Molecular Inorganic resulting in a large aquatic contamination. The conventional
Chemistry, Faculty of Chemistry, USTHB, El Alia, BP 32,
16111 Algiers, Algeria treatments destroy this molecule, but not enough to com-
2 ply with threshold required by the World Health Organiza-
Laboratory of Storage and Valorization of Renewable
Energies, Faculty of Chemistry, USTHB, El Alia, BP 32, tion (WHO). For this purpose, we have chosen the photo
16111 Algiers, Algeria catalysis as an efficient strategy for the MB oxidation by

13
Vol.:(0123456789)
 Journal of Materials Science: Materials in Electronics

exposition of ­MgFe2O4 to solar light. Nanoparticles were data were collected with a Specord 200 Plus spectropho-
used as photocatalysts, with 99 and 50% of MB degradation tometer equipped with an integrating sphere. The specific
after 60 min irradiation of UV light [19, 20]. surface area was evaluated by the BET method was using the
It is well known that the photocatalysis is efficient at low ASAP 2010 Micromeritics equipment and ­N2 gas in liquid
concentrations and can be used at the end of the treatment state (− 196 °C) as adsorbat. Before the measurement, the
chain. It is also an alternative energy to decrease the impact powder was degassed under vacuum at 150 °C overnight.
of fossil energy and greenhouse gases emission. According The equilibrium pH of a solution containing an excess
to WHO, the MB concentration does not exceed 0.4 ppm in powder in suspension permitted to determine the point
water. To this effect, we study the photocatalysis by varying of zero charge (pzc = 11.3). For the transport properties,
the concentration of MB, pH and catalyst dose. ­MgFe2O4 the powder was pressed into discs (∅ = 13  mm, thick-
fulfills the photo-electrochemical conditions i.e. friendly ness ~ 1  mm) and then sintered at 950  °C to get good
environmental characteristics, a chemical inertness and a mechanical properties (compactness ~ 90%). The electrical
forbidden of ~ 2 eV, permitting the conversion of half of the conductivity was measured by the two probes technique
solar light. Indeed, the solar energy meets a high demand in using GW Instek (GDM 8255A) equipment, the pellets was
the energy conversion and the photo-catalysis is an environ- sandwiched between two copper electrodes and heated up
mentally friendly alternative for the water treatment. Moreo- to 420 °C. For the electrochemical measurement, the elec-
ver, the dyes are toxic by themselves and weaken the light trical contact was realized with copper wire onto the back
penetration in water, thus disturbing the photosynthesis for pellet after putting conductive silver paint; then the pellet
concentrations as low as 5 mg L ­ − 1. In this optic, the present was encapsulated in a glass holder and isolated with epoxy
contribution aims at determining the physical and electro- resin. The electrochemical analysis was carried out in KOH
chemical properties of ­MgFe2O4. As application, the spinel (0.1 M) solution under ­N2 bubbling in a three electrodes cell,
is successfully tested for the photo degradation of methylene with ­MgFe2O4 working electrode, Pt counter electrode and a
blue (MB) under sunlight. saturated calomel electrode (SCE). The potential was moni-
Unlike other spinels which exhibit p-type behaviour, tored by PGZ 301 potentiostat (Radiometer), the intensity-
­MgFe2O4 is a narrow n-type semiconductor with a valence potential J(E) curves were plotted at a scan rate of 10 mV
band anodic enough to generate •OH radicals responsible of ­s−1; the capacitance measurement was done at a frequency of
the MB under solar light. The energy band diagram, estab- 10 kHz. The electrochemical impedance spectroscopy (EIS)
lished on the base of physical and photo-electrochemical was studied in the range ­(10−3–105 Hz), both in the dark and
characterizations, confirm that OH∙ is responsible of the MB under illumination (tungsten lamp, 200 W) after stabilization
photodegradation. of the open circuit potential ­EOCP (− 0.41 V).
The photocatalysis is efficient at the end of treatment and
is used as tertiary treatment; it was performed in double
2 Experimental wall batch reactor using methylene blue as reaction test. The
photo activity was studied in a Pyrex reactor equipped with
The photo catalytic performance is dependent on the syn- a cooling system; the temperature was maintained constant
thesis conditions and is considerably enhanced by using sol (25 ± 1 °C) thanks to a thermo stated bath. Before starting
gel route, which allow to get, a large specific surface areas tests, the solution was purged of air by bubbling through
i.e. small crystallites size. So, we adopt this method to syn- nitrogen. The reactor was directly exposed to solar light irra-
thesize the spinel M­ gFe2O4. Stoichiometric mixture of Mg diation (830 mW c­ m−2). The photo-catalytic experiments
­(NO3)9(H2O) (Biochem, 98%) and Fe(NO3)9(H2O)3 (Merck, were realized in stirred powder suspension under magnetic
98%) in a molar rapport (Mg/Fe: ½) was dissolved in dis- agitation at ambient temperature. The MB photo-degrada-
tilled water, to which agar agar (1 g ­L− 1) was added. The tion was followed by plotting the UV–visible spectra of MB
mixture was heated at 70 °C under agitation until apparition (λmax = 665 nm).
of a gel. The solution was dehydrated and treated at 100
and 300 °C. The amorphous powder was ground in an agate
mortar and the thermal analysis was studied in a thermo ana- 3 Results and discussion
lyser (Setaram Lab Sys TG DTA). Finally, the powder was
fired at 800 °C with intermediate regrinding. The phase was 3.1 Characterization
identified by X-ray diffraction (XRD) using Cu Kα radia-
tion (λ = 0.154178 nm). Attenuated total reflection (ATR) The TG plot of the initial mixture after evaporation (Fig. 1)
analysis of the powder was recorded with a Becker Alpha T, shows small weight losses, the first one at 120 °C (D1)
while the microstructure was analyzed by scanning electron is attributed to water deshydratation while the loss (D2)
microscope (SEM, Phillips XL30). The diffuse reflectance at ~ 150  °C is due to the elimination of organic matter

13
Journal of Materials Science: Materials in Electronics

15 this surface is very close to that obtained by BET analysis

D4 (460 °C)
D3 (345 °C)
10
(2.91 ± 0.01 m2/g).
100
MgFe2O4 is an inverse ]spinel (Fig. 2 right) and 3+
can be
5 formulated as (Fe)td MgFe oc O4 ,where ­Mg2+ and F ­ e ions
[

occupy tetrahedral sites, while the half of ­Fe2+ are tetrahe-

Heath flow (µV)

0
TG (%)

90 drally coordinated, the tetragonal structure is not distorted

-5
due to the absence of Jahn Teller effect (­ Fe3+:t2g
3
− e0g ).The
Endo

-10 morphology of the powder was observed by SEM image

80
-15 (Fig. 3.) which shows a homogeneous distribution of grains
with different forms (spherical and elliptical) and various
D2 (156 °C) -20
70 D1 (120°C) sizes, the existence of agglomerates grains is due to ferro-
0 200 400 600 800 1000 magnetism of the ferrite ­MgFe2O4 and the presence of cavi-
Temperature (°C) ties at micrometric scale.
The ATR spectrum (Fig. 4.) exhibits peaks at 571 cm−1
Fig. 1  TGA/DSC curves for thermal decomposition of ­
MgFe2O4 which corresponds to stretching vibration of octahedral
­ in−1)
under nitrogen flux (100 mL m Fe-O, 479 and 442 cm−1 due to Mg-O elongation in octahe-
dral sites [22]. The angular deformation of water occurs at
~ 1630 cm−1, while the vibrations of OH groups are local-
(agar–agar gelling agent). The losses D3 (345 °C) and D4 ized at ~ 3440 cm−1.
(460 °C) are assigned to the decomposition of Mg- and Fe-
nitrates. The plateau region beyond 650 °C clearly indicates 3.2 Optical and transport properties
the spinel formation.
The XRD pattern of ­MgFe2O4 synthesized by sol gel The variation of the diffuse reflectance (%R) shows an
shows single phase with no impurities; all peaks (Fig. 2 intense reflection in the visible region (Fig. 5 left); the Tauc
left) are assigned to
−
spinel structure and indexed in a cubic relation (1) is used to determine the optical gap energy ­(Eg)
symmetry (SG: Fd3 m) with a lattice parameter of 0.8382 nm [23]:
close to that obtained elsewhere [21] and in agreement with
(𝛼h𝜈)m = Const × (h𝜈 − Eg ) (1)
the JCPDS Card No 36-0398. Assuming nonporous crystal-
lites with a spherical form, the size (L ~ 450 nm) is evaluated The direct transition (m = 2), was obtained from the plot
from the empirical relation {L = 0.94λ/(βcosθ)}, this should of (αhν)m versus the photon energy (hν). The extrapolation
lead to a specific surface area of 2.95 m2/g{= 6/(ρexp. L)}, β of the straight line (αhν)2 = 0 gives a gap E ­ g of 2.16 eV
is the broadening of the most intense peak XRD spectrum, (Fig. 5 right), a value close to that obtained elsewhere [24]

3000
(311)

2000
(440)
(220)

(511)
(400)

1000
(222)

(412)
(111)
Intensity (%)

0 10 20 30 40 50 60 70 80

80
JCPDS N° 00-036-0398

40

0 10 20 30 40 50 60 70 80
2θ(°)

Fig. 2  XRD pattern of ­MgFe2O4 and the JCPDS sheet below (left). Crystal structure of ­MgFe2O4.The Mg atoms in tetrahedral position within
yellow color and Fe atoms within the green color and octahedral position (right). (Color figure online)

13
 Journal of Materials Science: Materials in Electronics

Fig. 3  SEM microstructure of oxide at different magnifications

displacement requires a complementary energy of the pho-

100 non, which is less probable [26, 27].
The exponential variation of the electrical conductivity
80 (σ) versus reciprocal temperature is characteristic of semi-
Transmitance (%)

C -O conductor behavior:
60
Ea
40 M g -O σ = σ0 exp(− ) (2)
RT
20 The slope of the linear plot gives an activation energy
F e -O ­(Ea1) of 0.134 eV (Fig. 6), much higher than the thermal
0 energy kT (~ 26 meV at 300 K) indicating that only a small
3500 3000 2500 2000 1500 1000 500
-1
W a v e n u m b e r (c m ) part of the charge carriers contributes to the conduction.
The value E­ a1 is the energy of electron hopping between
Fig. 4  Infrared spectrum of oxide ­MgFe2O4 obtained by ATR method octahedral sites (­ Fe2+ ↔ Fe3+). Curiously and in contrast to
other spinels, ­MgFe2O4 is the only one that exhibits n type
conductivity, due to F ­ e2+ ions insertion in the crystal lattice.
and in agreement with the red colour of M ­ gFe2O4. The The low electron mobility µe (2 × 10−6 ­m2 ­V−1 ­s−1) calcu-
gap ­Eg corresponds to the electronic transition: ­Fe3+oct: lated from the relation (σ = n e µe), shows that the carriers
t2g → Fe2+oct: eg attributed to the crystal field splitting of charges move in a narrow conduction band deriving from
­Fe3+ in octahedral coordination [25]. A further indirect ­Fe3+: 3d orbital, beyond 360 K the increase of the activa-
transition (2.13 eV, m = 0.5) is assigned to lattice vibra- tion energy (0.44 eV) indicates a change in the transport
tion due to crystallographic defects, where the electron mechanism [28].

13
Journal of Materials Science: Materials in Electronics

Fig. 5  Diffuse reflectance spec-

trum (left) and determination of
­MgFe2O4 for direct transition
(left). Direct transition (m = 2),
obtained from the plot of (αhν)2
versus the photon energy hν
(right)

cm2) and the curve shows a good electrochemical stability,

the decrease current below − 1 V is due to water reduction
into hydrogen. The electronic bands of the semiconductor
can be deduced from the flat band potential ­(Efb); the latter
is reliable obtained from the capacitance measurement:
C−1 = C−1
dl
+ C−1
SC (3)
where ­Cdl and C ­ SC are respectively to the double layer and
space charge capacitances; Because of the low conductivity
of ­MgFe2O4, the parasitic inductance can be ignored. So,
the approximation ­CH > > CSC is valid and can be neglected
C−1
H
 . To determine the position of the electronic bands, we
have plotted the variation of the interfacial capacitance vs.
Fig. 6  Variation of the electrical conductivity of ­MgFe2O4 as a func- the applied potential:
tion of 1000/T ( )
2
C = (E − Efb ) (4)
−2
ϵϵo eND

3.3 Electrochemical properties where ε is the dielectric constant of ­MgFe2O4, εo the dielec-

tric constant of vacuum and e elementary charge. The extrap-
This study is initiated to elucidate the electrochemical olation of the straight line to the potential axis ­(C−2 = 0)
behaviour of M­ gFe2O4, to delimit its electro activity domain gives a potential E ­ fb of 0.27  V (Fig.  7 right). M
­ gFe2O4
and to determine different potential of involved redox cou- exhibits n-type character, evidenced by the positive photo
ple. The J(E) characteristic (Fig. 7 left) plotted in the dark current in the chrono-amperometric profile (Fig. 8 left),
exhibits a peak at ~ 0.77 V, corresponding to the couple F­ e3+/ and confirmed by the positive slope of the (­ C−2−E) curve.
Fe2+. The absence of peak in the reverse scan is assigned to The bending below 0.27 V is due to an increased capaci-
an irreversible process. The dark current is small (~ 1 µA/ tance related to the accumulation of electron/hole ­(e−/h+)

Fig. 7  J (V) Curve of the 4

2+ 3+
­MgFe2O4 in KOH (0.1 M) Fe /Fe
1,6
electrolyte (left) and the Mott– generation of H2
Schottky curve ­(C−2−V) of
­MgFe2O4 in a KOH solution 0 1,2
C (µF Cm )

(0.1 M) plotted at 10 kHz (right)

4
J(mA/cm )
2

-2

0,8
-4 Vbp =0,27 V
-2

0,4

-8 0,0
-2 -1 0 1 2 -1,0 -0,5 0,0 0,5 1,0
Potential (V) Potential (V)

13
 Journal of Materials Science: Materials in Electronics

Fig. 8  Chrono-amperometry 60 3.5
profile of ­MgFe2O4 with 20 s
switch on, switch off time dura- 3.0
tion (left). The impedance spec-
40 2.5
troscopy diagram of ­MgFe2O4

J( µA/cm²)

-Zi (kΩ cm2)

in KOH solution (0.1 M) 2.0
solution, under irradiation and
illumination 1.5 in the Dark
in the dark. Inset: the equivalent 20 under illumination
electrical circuit (right) dark 1.0

0.5
0
0 200 400 600 800 0.0
0 1 2 3 4 5
Time (Sec) Zr (k Ω cm2)

pairs while the plateau region above 0.67 V corresponds to carriers, corroborates the fast reduction at the interface
a depletion region. The electron density (­ ND = 1.94 × 1017 semiconductor/electrolyte.
­cm−3), calculated from the slope, reveals an oxide slightly The physical and electrochemical parameters (­ Eg, ­Ea and
doped with an extended depletion width (~ 220 nm): ­Efb) allow us to draw the energy band diagram of the junc-
tion ­MgFe2O4/electrolyte (Fig. 9) and to predict which radi-
cal is formed to contribute to the photoactivity:
( )0.5
2ϵϵo 𝛥V
W= (5)
eND EBC = 4.75 − eEfb − Ea (7)
W extend on several crystallite unit cells, ΔV is the opti- EBV = EBC − Eg (8)
mal band banding at the interface semiconductor electrolyte
The energy levels are pH-independent due to their cationic
(~ 0.5) which should give to a zero recombination [29].
character, 4.75 is energy of SCE with respect vacuum.
EIS permits a correlation between the morphology and
the electrical properties and the response as a function of
3.4 MB application
the perturbation frequency can reveal the internal dynamics.
In the dark, the Nyquist diagram (Fig. 8 right) reveals one
Currently, the solar energy is employed for both the energy
depressed semi-circle assigned to the bulk resistance ­(Rb). It
supply and environmental protection. In this regard, the
is centred below the real axis ­(Zreal), associated to existence
photocatalysis is an attractive alternative and the semicon-
of no ideal capacitor and the existence of a constant phase
ducting oxides are selected on the basis of their low cost,
element (CPE):
friendly characteristics, chemical stability and forbidden
Zc = [C(jw)n ]−1 , (n = 1−2q∕p) (6) band, conditions fulfilled by the spinel ­MgFe2O4. The oxide
With0 ≤ n ≤ 1 , CPE is attributed to surface states and formed with atoms of low electronegativity, is promising in
roughness of the electrode [30]. The minimal pulsation (ω) photocatalysis owing to the shift of the flat band potential
is used to determine the life time of electrons (τ = ω min−1). toward the cathodic side where the electrons in the conduc-
The offset near the origin is due to electrolyte resistance ­(Rel) tion band possess a high reducing ability. Therefore, the con-
and does not vary upper irradiation. An electrical equivalent duction band is cathodic enough to generate an interfacial
circuit (Fig. 8 right, Inset) is established by using the Zview band bending for the separation of (e−/h+) pairs.
software. The kinetic parameters are gathered in Table 1 The hole transfer at the interface SC/solution occurs ener-
after circular regression fitting of the electrochemical param- getically and the ability of a semiconductor material to drive
eters in the dark and under illumination. The decrease of the ­O2•− formation, is governed by the potential of •OH/H2O
the resistance ­Rb under light confirms the semiconducting ­(EOH•/H2O = 2.04) [31], compared to the valence band (VB)
behaviour while the decrease of the short life time of charge which is favourable in this case. On the other hand, the for-
mation of O ­ 2•− is unfavorable due to evolution of O­ 2/H2O

Table 1  Impedance properties of M
­ gFe2O4 in KOH (0.1 M) solution
Electro chemical parameters Efree (V) Rel (Ω ­cm2) Rb (Ω ­cm2) θ (°) CPE(µF/cm2) N fmin (Hz) t (s)

In the dark − 0 .626 79.19 5.387 − 14.9 525.8 0.83 0.42 0.71
Under illumination − 0.277 78.41 4.929 − 15.6 574.6 0.8 0.63 0.27

13
Journal of Materials Science: Materials in Electronics

Fig. 9  Energy diagram of the Energy (eV) Potential (VSCE)

junction ­MgFe2O4/electrolyte

0 -4.75

Conduction band (Fe3+ : eg)

ECB =- 4.60 0.131

Ea = 0.139 eV 0.27

Eg = 2.13 eV Products
Fe3+ : 3d5

OH•

H2O
EVB = -6.73 2.281
Valence band (Fe2+ : teg)

potential which changes by − 0.059 V p­ H−1. Indeed, at neutral Co and C

­ t are respectively the concentration of MB solu-
pH, the potential of CB is less cathodic than the potential o­ fO2/ tions before and after 2 h of solar irradiation. The decreased
O2•− couple and the attachment of MB on the catalyst surface absorbance over illumination time is due to MB mineraliza-
should favor the electronic transfer. tion by •OH radicals through a valence band process:
The photo degradation yield (η) is proportional to the
absorption coefficient (αλ) when both the space charge region
MgFe2 O4 + h𝜈 → h+VB + e−CB (10)
and the diffusion length are smaller than the light penetration h+VB + OH− →∙ OH (11)
(α−1) and higher than crystallite size (d), such conditions are
encountered in moderate doped oxides. The low conductivity h+VB + H2 O →∙ OH + H+ (12)
of the spinel extends the depletion length, where the formation
of (e−/h+) occurs (Fig. 10 left) gives the UV–Visible spectra ∙OH + H2 O → Products (13)
evolution with time course under solar irradiation and obeys The mechanism of photo degradation was resumed in dif-
to a first order reaction with a correlation factor ­(R2) of 0.94 ferent reactions cited above. It is helpful to outline that the
(Fig. 10 right). The yield (η) of photo degradation reaches photoactivity decreases only slightly after the second cycle
80%, calculated from the relation: (< 3%). We have observed a slight decomposition (~ 2%) of
( ) the photocatalyst (SM 3).The work is continuing with the
C0 − Ct × 100
η= (9)
C0

Fig. 10  MB photo catalytic Initial

degradation spectra for every Yield around of 80%
15 min
45
0
2
15 min at neutral pH, 25 °C 75 R = 0.94
2
and mass concentration of 105
120
20 mg/40 mL (right), and kinet-
Absorbance

ics degradation after 2 h of sun

Ln C/Co

light irradiation (left) -1

1

0 -2
200 400 600 800 0 50 100 150
Wavelength λ (nm) Time (min)

13
 Journal of Materials Science: Materials in Electronics

degradation of other dyes like methyl orange. The results are 8. S. Muhammad, J. Liu, A. Zahid, S. Imran, M.F. Warsi, P. Riffat,
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