Enhanced photocatalytic performance by Y-doped BiFeO3 particles derived from MOFs precursor based on band gap reduction and oxygen vacancies

Article abstract of DOI:10.1002/aoc.6113

In order to improve the photocatalytic performance of BiFeO₃, we prepared BiFeO₃ nanoparticles doped with different molar concentrations of Y by thermal decomposition of MOFs precursor. The samples were characterized by XRD, TG, FESEM, XPS, UV-vis, and PL. The results of XRD and XPS reveal that Y³⁺ have been successfully incorporated into BiFeO₃ lattice. FESEM and UV-vis results reveal that Y doping leads to a decrease in BiFeO₃ particle size and band gap. PL shows that the recombination rate of photogenerated electron hole pairs of Bi_0.95Y_0.05FeO₃ is the lowest. The influences of Y doping content on photocatalytic activity of BiFeO₃ have been investigated. The results show that the best photocatalytic activity is Bi_0.95Y_0.05FeO₃. Compared with pure BiFeO₃, Bi_0.95Y_0.05FeO₃ increased the degradation rate of MO by 1.3 times in 120 min. This may be due to the larger light response range and the lower photogenerated electron hole pairs recombination rate.

Full text of DOI:10.1002/aoc.6113

Received: 24 June 2020
DOI: 10.1002/aoc.6113
Revised: 1 October 2020
Accepted: 22 November 2020
F U L L P A P E R
Enhanced photocatalytic performance by Y-doped BiFeO3
particles derived from MOFs precursor based on band gap
reduction and oxygen vacancies
Zhendong Li1 | Li Cheng1 | Ke Zhang1 | Zhenhua Wang1,2
1School of Metallurgy and Materials
In order to improve the photocatalytic performance of BiFeO3, we prepared
BiFeO3 nanoparticles doped with different molar concentrations of Y by ther-
mal decomposition of MOFs precursor. The samples were characterized by
XRD, TG, FESEM, XPS, UV-vis, and PL. The results of XRD and XPS reveal
that Y3+ have been successfully incorporated into BiFeO3 lattice. FESEM and
UV-vis results reveal that Y doping leads to a decrease in BiFeO3 particle size
and band gap. PL shows that the recombination rate of photogenerated elec-
tron hole pairs of Bi0.95Y0.05FeO3 is the lowest. The influences of Y doping con-
tent on photocatalytic activity of BiFeO3 have been investigated. The results
show that the best photocatalytic activity is Bi0.95Y0.05FeO3. Compared with
pure BiFeO3, Bi0.95Y0.05FeO3 increased the degradation rate of MO by 1.3 times
in 120 min. This may be due to the larger light response range and the lower
photogenerated electron hole pairs recombination rate.
Engineering, Chongqing University of
Science and Technology, Chongqing,
China
2Chongqing Key Laboratory of Nano/
Micro Composite Materials and Devices,
Chongqing, China
Correspondence
Zhenhua Wang, Chongqing Key
Laboratory of Nano/Micro Composite
Materials and Devices, Chongqing 401331,
China.
Email: zhenhuaw@mail.ustc.edu.cn
Funding information
Leading Talents of Scientific and
Technological Innovation in Chongqing,
Grant/Award Number:
CSTCCXLJRC201919; Chongqing
Research Program of Basic Research and
Frontier Technology, Grant/Award
Numbers: CSTC2018jcyjAX0416,
cstc2019jcyj-msxmX0071; Scientific and
Technological Research Program of
Chongqing Municipal Education
Commission, Grant/Award Numbers:
KJQN201801509, KJZD-M201901501
K E Y W O R D S
MOFs precursor, photocatalytic activity, Y-doped BiFeO3 nanoparticles
1 | INTRODUCTION
Because of the small band gap (2.2–2.5 eV), BiFeO3
has been considered as
a potential visible light
In recent years, due to the advantages of no secondary pol-
lution, high efficiency, and stability, photocatalytic oxida-
tion technology has been widely used in the treatment of
organic dye wastewater.[1,2] At present, some high effi-
ciency oxide semiconductors have been reported, such as
ZnO, TiO2, and SnO2.[3–5] Even though these materials
have been proved to be outstanding photocatalysts for the
degradation of dye wastewater, these large band gap oxide
semiconductors only use ultraviolet light, which limits
their application. Therefore, it is of great significance to
find other highly activity visible light catalysts.
photocatalyst.[6,7] So far, there have been a lot of reports
about improving the optical, ferroelectric, and ferromag-
netic properties of BiFeO3 by doping metal ions at A site
or B site or both A and B sites in the BiFeO3 lattice. At
present, metal ion doping has been considered as one of
the effective methods to enhance the photocatalytic per-
formance of BiFeO3,[8–12] especially rare earth elements,
because they have special 4f electronic structure, which
can promote the separation of electron–hole pairs.[13]
Generally, the rare earth elements are all +3 valence, and
their ionic radius is similar to Bi3+, making it possible for
Appl Organomet Chem. 2020;e6113.
wileyonlinelibrary.com/journal/aoc
© 2020 John Wiley & Sons, Ltd.
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https://doi.org/10.1002/aoc.6113

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LI ET AL.
the rare earth elements to easily replace Bi3+. For exam-
ple, Hu et al. studied that the photocatalytic performance
was improved by doping Sm, which was mainly due to
visible light absorption enhancement and the effective
separation of photogenerated electrons and holes.[14] It
2.2 | Preparation of the photocatalysts
Preparation process of Bi1−xYxFeO3 (x = 0, 0.005, 0.01,
0.05, 0.1, 0.2) photocatalysts: The photocatalysts
Bi1−xYxFeO3 (x = 0, 0.005, 0.01, 0.05, 0.1, 0.2) were
prepared as follows: first, dissolve 20-mmol K3[Fe(CN)6]
in 40-ml distilled water to form solution A; 20-mmol
mixture of Y(NO3)3ꢀ6H2O and Bi(NO3)3ꢀ5H2O with
stoichiometric ratio were dissolved in 40-ml nitric acid
(3 mol/L) to form solution B. Next, add solution B into
solution A and stir continuously. After stirring for
30 min, the obtained coffee color solution was for 24 hr
at room temperature. Next, centrifuge the coffee color
precipitate (wash with absolute ethanol) and store in an
oven for a period of time to obtain the MOFs precursor
Bi1−xYx[Fe(CN)6]ꢀ4H2O. Bi1−xYxFeO3 particles were
prepared by annealing Bi1−xYx[Fe(CN)6]ꢀ4H2O. On the
basis of the TG curves of Bi1−xYx[Fe(CN)6]ꢀ4H2O, the
MOFs precursor were put into a tubular furnace, heated
from room temperature to 500ꢁC at 5ꢁC/min, and then
kept for 5 hr. Finally, cool it to room temperature to
get Bi1-xYxFeO3 particles.
should be noted that the Y3+ ion radius is less than Bi3+
.
In other reports, Y has been proved to be an effective
doping element to enhance the dielectric and magnetic
[15–18]
properties of BiFeO3.
Therefore, we predict that
replacing Bi with an appropriate content of Y may also
improve the photocatalytic activity of BiFeO3.
Recently, metal-organic frameworks (MOFs) have
become a research focus because of its porosity and high
surface area.[19–22] At the same time, it is also a precursor
for the preparation of nano-porous materials.[23,24] Our
group has successfully prepared smaller band gap BiFeO3
by decomposing the MOFs precursor Bi[Fe(CN)6]ꢀ4H2O
by thermal decomposition and found that Co-doping at B
site also promoted the photocatalytic activity of
BiFeO3.[25,26] In order to explore the effect of Y-doped at A
site on the photocatalytic activity of BiFeO3, in this work,
we synthesized Bi1-xYxFeO3 by calcining MOFs precursor
Bi1−xYx[Fe(CN)6]ꢀ4H2O, as shown in Figure 1. And the
effects of the Y3+ dopant concentration on the phase, mor-
phology, optical absorption and photocatalytic activity of
BiFeO3 were systematically studied in this paper.
2.3 | Characterization
The crystal structures were analyzed by X-ray diffraction
(Rigaku D/max2400, λ = 1.54178 Å) with Cu Kα radia-
tion source. The morphologies were tested by scanning
electron microscopy (JSM-7800F). The thermogravimetric
test was carried out with STA 449 F1. The chemical state
of the sample was tested by the X-ray photoelectron spec-
troscopy (VSW, excitation energy 1486.6 eV) with Al Kα
source. The light absorption test was carried out with
UV–vis spectrophotometer (Hitachi U-3900). The PL
spectra were tested by fluorescence spectrophotometer
(Hitachi FL4500).
2 | EXPERIMENTAL
2.1 | Materials
Bismuth nitrate (Bi(NO3)3ꢀ5H2O), yttrium nitrate (Y
(NO3)3ꢀ6H2O), potassium ferricyanide (K3[Fe(CN)6]), nit-
ric acid (HNO3), methyl orange (C14H14N3SO3Na), and
anhydrous ethanol are analytical grade. Distilled water
was used in all experiments.
FIGURE 1 Synthesis process of Bi1−xYxFeO3 photocatalyst derived from Bi1−xYx[Fe(CN)6]ꢀ4H2O

LI ET AL.
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2.4 | Photocatalysis test
In order to successfully prepare Bi1−xYxFeO3, the
thermal decomposition behavior of the series Bi1−xYx[Fe
(CN)6]ꢀ4H2O was studied by TG analysis, as shown in
Figure 3. The TG curves indicate that the weight loss
occurs mainly in two stages from room temperature to
500ꢁC. The first weight loss is between room temperature
and 180ꢁC, which corresponds to the loss of crystal water
in the precursors of MOFs. The second weight loss is
between 180ꢁC and 500ꢁC, mainly due to the decomposi-
tion and oxidation of cyanide, and simultaneously forma-
tion of oxides Bi2O3, Fe2O3, Y2O3, and BiFeO3. Finally,
The photocatalytic activity of Bi1−xYxFeO3 was studied by
degradation of methyl orange (MO) with 300-W Xe lamp
(λ = 390–770 nm). First of all, 100 mg Bi1−xYxFeO3 was
added to 100-ml MO solution (10 mg/L) and stirred for
30 min under dark conditions to reach adsorption equi-
librium. Then, irradiate with visible light and take 4 ml
of suspension every 20 min. Finally, the concentration of
MO was measured by UV–vis spectrophotometer, and
the photocatalytic degradation efficiency can be calcu-
lated by the following formula:
[27]
Bi2O3, Y2O3, and Fe2O3 react to form Bi1−xYxFeO3.
The possible mechanism of thermal decomposition can
be expressed by the following equation:
D = ðC0 – CtÞ=C0 × 100%
ð1Þ
where C0 (C0 = 10 mg/L) represents the initial con-
centration of MO and Ct represents the concentration of
MO after light time t.
3 | RESULTS AND DISCUSSION
Figure 2 is the XRD patterns for the Bi1−xYx[Fe(CN)6]ꢀ
4H2O complexes. The XRD patterns of all the MOFs pre-
cursor are very similar, and the XRD peaks corresponds
to Bi[Fe(CN)6]ꢀ4H2O (PDF#80-0961, orthorhombic cell,
space group: Cmcm). The relationship between unit cell
volume and Y doping is shown in Figure 2 (inset). It is
obvious that the decrease of cell volume with the increase
of x (Y content), since the Y3+ ion radius less than that of
Bi3+ in this precursor, as reported by Singh et al.[18]
FIGURE 3 The TG curves of Bi1−xYx[Fe(CN)6]ꢀ4H2O
FIGURE 2 XRD patterns of Bi1−xYx[Fe
(CN)6]ꢀ4H2O; the inset is the variation of cell
volume with Y-doping content

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LI ET AL.
The first stage:
constants and cell volumes of Bi1−xYxFeO3 are shown in
Table 1. It can be seen that the lattice constant and cell vol-
ume of Y-doped BiFeO3 are slightly lower than that of pure
BiFeO3, indicating that the lattice distortion of BiFeO3 is
caused by doping. It is worth noting that the appearance of
the Bi7.5Y0.5O12, YFe2O4, Bi2Fe4O9, and Bi2O3 impure
phases is observed. When Y doping is low, there is mainly
Bi2O3 as Bi is easy to volatilize.[28] It has also been men-
tioned in other literatures that other impure phases con-
taining yttrium would appear when the doped Y increases
and exceed the solid solubility.[16,29]
Â
Ã
Â
Ã
Bi1−xYx FeðCNÞ6 ꢀ4H2OðsÞ ! Bi1−xYx FeðCNÞ6 ðsÞ + 4H2OðgÞ
ð2Þ
The second stage:
Â
Ã
3
2
1
2
1−x
Bi1−xYx FeðCNÞ6 ðsÞ + O2ðgÞ ! Bi1−xYxFeO3ðsÞ +
Bi2O3ðsÞ
4
x
1
+
Y2O3ðsÞ + Fe2O3ðsÞ + 3ðCNÞ2ðgÞ
4
4
FESEM image is shown in Figure 5; obviously, all the
samples are made of very fine spherical particles. As the
gas released during the calcination of the precursor, these
particles were gathered together to form porous struc-
ture.[30] This structure facilitates the adsorption of reac-
tant molecules and provides more active sites. For pure
BiFeO3, the particles' size is roughly around 100 nm.
ð3Þ
1
2
1−x
4
x
1
4
Bi1−xYxFeO3ðsÞ +
! Bi1−xYxFeO3ðsÞ
Bi2O3ðsÞ + Y2O3ðsÞ + Fe2O3ðsÞ
4
ð4Þ
On the basis of the TG curves of Bi1−xYx[Fe(CN)6]ꢀ
4H2O, the MOFs precursor was calcined at 500ꢁC for 5 hr
to obtain Bi1−xYxFeO3 nanoparticles. Figure 4 shows the
XRD pattern of the Bi1−xYxFeO3; all diffraction peaks cor-
respond to rhombic perovskite structure (PDF#82-1254,
space group: R3c). Since the Y3+ ion radius (1.04 Å) is
smaller than that of Bi3+ (1.17 Å), all the peaks gradually
move to higher angles with the increase of Y doping con-
centration, and the double peaks of (104) and (110) split
into four peaks when x = 0.2. The changes of the above
XRD peaks are similar to those reported by Medina
et al.,[16] which indicates that some Y ions replace Bi ions
and are successfully doped into BiFeO3 lattice. The lattice
TABLE 1 The lattice parameters of Bi1−xYxFeO3 (calculated
from Jade 6.5)
Lattice constants (Å)
Bi1−xYxFeO3
x = 0
a
c
Volume (Å3)
373.83
5.5792
5.5672
5.57778
5.57993
5.57687
5.57467
13.86607
13.82807
13.83837
13.84961
13.82083
13.82429
x = 0.005
x = 0.01
x = 0.05
x = 0.1
371.16
372.85
373.44
372.26
x = 0.2
372.06
FIGURE 4 The XRD patterns of Bi1−xYxFeO3

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FIGURE 5 FESEM images of the Bi1−xYxFeO3 with different Y doping contents (a) x = 0, (b) x = 0.005, (c) x = 0.01, (d) x = 0.05,
(e) x = 0.1, (f) x = 0.2
Compared with pure BiFeO3, the particles' size of Y-
light leads to the band gap transitions.[34] According to
doped BiFeO3 decreases to about 50 nm; it is less than
the absorption spectrum data, the band gap value is cal-
culated by[35]
[31–33]
other reported Y-doped BiFeO3.
This indicates that
appropriate Y-doping of BiFeO3 can reduce the particle
size, which is conducive to photocatalytic reaction.
À
Á
n
ðαhνÞ = B hν – Eg
ð5Þ
The optical absorption characteristic of photocatalysts
was studied by UV–vis spectrophotometry, which are
shown in Figure 6. As shown in Figure 6a, all the
photocatalyst show strong light absorption ability in visi-
ble light region (400–800 nm), indicating that Bi1
−xYxFeO3 can perform photocatalytic reaction in visible
light. It is noteworthy that with the increase of Y doping,
the more obvious red shift that the samples absorption
spectra showing, especially for the samples x = 0.1 and
x = 0.2. In addition, all photocatalysts show a steep
absorption edge, which indicates that the absorption of
Here, α is the absorbance, h is the Planck's constant, ν
is the optical frequency, Eg is the band gap, and B is the
constant. The Eg is obtained by extrapolating a line on the
photon energy from the (αhν)2 plot to the point where it
becomes zero, as shown in Figure 6b. The band gap energy
of BiFeO3 nanoparticles is 2.12 eV, which is quite
similar to previous reports.[6,14,36] The band gaps of the
Bi1−xYxFeO3 (x = 0.005, 0.01, 0.05, 0.1, 0.2) samples are
FIGURE 6 (a) UV-vis absorption spectra and (b) (αhν)2 versus (hν) curves graph of all samples

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LI ET AL.
estimated to be 2.15, 2.13, 2.09, 2.04, and 2.02 eV, respec-
tively. The above results show that proper Y doping can
decrease the band gap of BiFeO3. The most common defect
of BiFeO3 is oxygen vacancy, which is mainly caused by a
defect near the conduction band.[37] Thus, the band gap of
BiFeO3 decreases with Y high concentration doping.
529.2, 530.7, and 532.1 eV, respectively, represents lattice
oxygen, oxygen vacancy and chemically adsorbed
oxygen,[39] and the ratio of O1 (lattice oxygen) to O2
(oxygen vacancy) to O3 (chemisorbed oxygen) in
Bi0.95Y0.05FeO3 is 61:21:18. In the process of photo-
catalytic reaction, oxygen vacancies may be the capture
center of electron, which can effectively inhibit the
recombination of electron-hole pairs.[40–42] The mean-
In order to study the valence state of Fe and the char-
acteristics of oxygen element, the XPS spectrum of
Bi0.95Y0.05FeO3 was further investigated, as shown in
Figure 7. Figure 7a shows the presence of four elements
Bi, Y, Fe, and O in the sample. In order to elucidate the
chemical nature of Y in Bi0.95Y0.05FeO3, we analyzed the
XPS spectra of the Y 3d peak, as shown in Figure 7b. The
main features occurred at 158.2 eV is the peak position of
Y 3d5/2, which indicates the presence of +3 valency
Y. The coexistence of Fe2+ and Fe3+ in the sample is
shown in Figure 7c. The peak at 709.8 eV is assigned to
−
time, the ꢀO2 free radicals that promote the oxidation of
organics are generated, as shown in Equation 6–10[43–45]
:
e− + O2 ! ꢀO2
O2 − + H2O ! ꢀHO2 + OH−
HO2 + H2O ! H2O2 + ꢀOH
H2O2 ! 2ꢀOH
ð6Þ
ð7Þ
−
ð8Þ
Fe2+, and the peak at 711.8 eV is assigned to Fe3+ [38]
The
.
ratio of Fe2+ to Fe3+ in Bi0.95Y0.05FeO3 is 44:56, and the
lower Fe2+ concentration may also be evidence of oxygen
vacancy. Figure 7d shows the O 1s spectrum, located near
ð9Þ
OH + Dye ! Degradation products
ð10Þ
FIGURE 7 XPS spectra: (a) Overall core level, (b) Y 3d, (c) Fe 2p, and (d) O 1s for the Bi0.95Y0.05FeO3 sample

LI ET AL.
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The photocatalytic activity of Bi1−xYxFeO3 is shown
in Figure 8a. The photocatalytic degradation rate of MO
increased with the increase of illumination time. In addi-
tion, proper Y doping can enhance photocatalytic activity
of BiFeO3. Especially, the degradation of Bi0.95Y0.05FeO3
reached 69.3% within 120 min, exhibiting the best photo-
catalytic performance. Interestingly, when the Y doping
content increase from 0% to 5%, the photocatalytic degra-
dation rate of MO reaches the best value. As the Y con-
tent continues to increase, the degradation efficiency of
MO begins to decrease. Photocatalytic MO conforms to
the first-order reaction kinetics, and the photocatalysis
rate constant can be expressed as follows:
ln ðCt=C0Þ = −kt
ð11Þ
FIGURE 9 PL spectra of Bi1−xYxFeO3 photocatalysts
where k is the photocatalysis rate constant. Figure 8b
is the relationship between ln (Ct/C0) and time t. The
photocatalysis rate constants of Bi1−xYxFeO3 (x = 0,
0.005, 0.01, 0.05, 0.1 and 0.2) are to be 0.00208, 0.00487,
0.00608, 0.00996, 0.00926, and 0.086 min−1, respectively.
It is well known that PL spectrum is to study optical
and electronic properties of semiconductors, and photo-
catalytic activity is also affected by the competition
between recombination and the charge separation pro-
cess.[46] Figure 9 is the PL spectrum of the Bi1−xYxFeO3
photocatalysts measured at room temperature. The previ-
ous studies showed that the lower the photoluminescence
intensity, the lower the recombination rate of electrons
and holes, so the strong photocatalytic activity can be
obtained. Doping Y is most likely to play a key factor in
electron hole pair recombination. In this work,
Bi0.95Y0.05FeO3 showed the weakest PL peak and thus
showed the best photocatalytic activity.
(Figure 6), the concentration of the generated photo-
carriers is higher, which enhances the photocatalytic
performance. At the same time, since the particle size
of the Y-doped sample is smaller than that of the pure
BiFeO3 (Figure 5), the effective contact area with visible
light increases during photocatalytic process, which is
also important to improve the photocatalytic perfor-
mance. Interestingly, with the continuous increase of Y
content, the degradation efficiency of MO begins to
decrease (Figure 8). Actually, there is an optimal con-
tent of Y3+ doping in Bi1−xYxFeO3 particles to most
effectively separate electron-hole pairs, which can be
explained by the space charge layer, and the doping
concentration affects the thickness of the space charge
layer, as shown in following[47]
:
ꢀ
ꢁ
1=2
2εε0Vs
eNd
Compared with the pure BiFeO3, the Y-doped sam-
ples enhance the absorption in the visible range
W =
ð12Þ
FIGURE 8 (a) The photocatalytic degradation efficiency of all samples; (b) the plots of ln (Ct/C0) versus time t of all samples

8 of 9
LI ET AL.
where W is the space charge layer thickness, ε is the
static dielectric constants, ε0 is the vacuum static
dielectric constant, Vs is the surface potential, Nd is
the number of dopant donor atoms, and e is the elec-
tronic charge. It can be seen clearly that W decreases
with the increase of Nd. In this work, when the when
Y doping concentration increases by 5%, the space
charge layer thickness is basically equal to the depth
of light penetration, thus effectively separate the
electron-hole pairs in the region.[48] However, when
the content of Y doping exceeds its optimal value, the
penetration depth of light is greater than the space
charge layer. In this case, the recombination of
electron-hole pairs becomes easier, which reduces the
photocatalytic performance of the photocatalyst.[49]
DATA AVAILABILITY STATEMENT
The data that support the findings of this study are avail-
able from the corresponding author upon reasonable
request.
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In this paper, Bi1−xYxFeO3 nano photocatalyst is pre-
pared by calcination MOFs precursor Bi1−xYx[Fe(CN)6]ꢀ
4H2O. Most photocatalyst is composed of spherical par-
ticles of about 50 nm. The Bi0.95Y0.05FeO3 exhibited
the best photocatalytic activity, compared with pure
BiFeO3, Bi0.95Y0.05FeO3 increased the degradation rate
of MO by 1.3 times in 120 min. This may be because
the larger light response range and the lower
photogenerated electron-hole pairs recombination rate.
Moreover, with the increase of doping content, the
penetration depth of light is greater than the space
charge layer; the recombination of electron-hole pairs
becomes easier, which reduces the photocatalytic per-
formance of the photocatalyst. This work provides a
new method for the preparation of BiFeO3 and pro-
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This work was supported by the Scientific and
Technological Research Program of Chongqing Munici-
pal Education Commission (KJQN201801509 and KJZD-
M201901501), the Chongqing Research Program of Basic
Research and Frontier Technology (CSTC2018jcyjAX0416
and cstc2019jcyj-msxmX0071), and the Leading Talents
of Scientific and Technological Innovation in Chongqing
(CSTCCXLJRC201919).
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How to cite this article: Li Z, Cheng L, Zhang K,
Wang Z. Enhanced photocatalytic performance by
Y-doped BiFeO3 particles derived from MOFs
precursor based on band gap reduction and oxygen
vacancies. Appl Organomet Chem. 2020;e6113.
https://doi.org/10.1002/aoc.6113
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