J Mater Sci: Mater Electron (2014) 25:2463–2469
DOI 10.1007/s10854-014-1896-0
Enhanced photocatalytic activity of BiFeO3 particles by surface
decoration with Ag nanoparticles
L. J. Di • H. Yang • G. Hu • T. Xian •
J. Y. Ma • J. L. Jiang • R. S. Li • Z. Q. Wei
Received: 18 February 2014 / Accepted: 21 March 2014 / Published online: 30 March 2014
Ó Springer Science+Business Media New York 2014
Abstract BiFeO3 particles with different morphologies
and sizes were synthesized via a hydrothermal process,
where the morphology and size was tailored by using dif-
ferent KOH concentrations in precursor solution. The
samples prepared at n(KOH) = 3, 4.5, 6, and 7.5 M are
composed, respectively, of octahedron-shaped particles
(500–600 nm), cube-like particles (200–500 nm), irregular
spherical agglomerates (9–16 lm) formed from disk-like
grains with diameter of 1.4–2.8 lm and thickness of
0.2 lm, and cuboid-shaped particles with length-to-width
ratio of 1.4:1–3.5:1 and width size ranging from 80 to
280 nm. Ag nanoparticles were deposited on the surface of
BiFeO3 particles by a chemical reduction method to pro-
duce Ag@BiFeO3 nanocomposites. The photocatalytic
activity of prepared samples was evaluated by degrading
rhodamine B under simulated sunlight irradiation. It is
demonstrated that Ag-decorated BiFeO3 particles exhibit
an enhanced photocatalytic activity compared to bare Bi-
FeO3 particles. This can be explained by the effective
transfer of photogenerated electrons from the conduction
band of BiFeO3 to Ag nanoparticles and hence increased
availability of holes for the photocatalytic reaction.
Hydroxyl radicals were detected by the photoluminescence
L. J. Di  H. Yang  T. Xian  J. L. Jiang  R. S. Li  Z. Q. Wei
School of Science, Lanzhou University of Technology,
Lanzhou 730050, People’s Republic of China
H. Yang (&)  T. Xian  J. Y. Ma  Z. Q. Wei
State Key Laboratory of Gansu Advanced Non-ferrous Metal
Materials, Lanzhou University of Technology, Lanzhou 730050,
People’s Republic of China
e-mail: hyang@lut.cn
G. Hu
Chengdu Compressor Plant, CNPC Jichai Power Equipment
Company, Chengdu 610100, People’s Republic of China
technique using terephthalic acid as a probe molecule and
are found to be produced over the irradiated BiFeO3 and
Ag@BiFeO3 photocatalysts; especially, an enhanced yield
is observed for the latter.
1 Introduction
With the rapid development of global industrialization,
environmental pollution and energy shortage have become
two impending problems that confront mankind today.
Semiconductor-based photocatalysis has received consid-
erable attention as an ideal green technology for solving the
intractable environmental and energy problems [1, 2]. TiO2
is one of the most popular photocatalysts, exhibiting
powerful capabilities for photocatalytically degrading all
types of organic pollutants completely into harmless inor-
ganic substances and splitting water into hydrogen and
oxygen. However, TiO2 is active only under irradiation of
ultraviolet (UV) light at wavelengths below 390 nm due to
its wide bandgap energy of *3.2 eV. It is known that
visible light accounts for *45 % of the energy in the solar
spectrum while only a small fraction of *5 % is in the UV
portion. In order to efficiently take advantage of solar
energy to drive photocatalytic reaction, the development of
visible-light responsive photocatalysts has been considered
to be indispensable.
Bismuth-based oxide semiconductors are known to be
an important class of visible-light responsive photocata-
lysts. This class of semiconductors generally have a mod-
erate bandgap energy centered around 2.0 eV and are able
to absorb visible light over a wide range of wavelengths.
Bismuth ferrite (BiFeO3) with a rhombohedrally distorted
perovskite structure is one of the outstanding bismuth-
based oxide semiconductors. Besides its famously-known
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multiferroic properties [3–5], BiFeO3 also exhibits a pro-
nounced photocatalytic activity toward the degradation of
various organic dyes under visible-light irradiation such as
reactive black 5 (RB5) [6], rhodamine B (RhB) [7, 8],
congo red (CR) [9] and methyl orange (MO) [10]. Fur-
thermore, BiFeO3 nanowires decorated with Au nanopar-
ticles can be used as highly efficient photocatalysts for
water splitting [11]. Generally, the photocatalytic activity
of semiconductors depends on numerous factors. Promot-
ing the separation of photogenerated electron–hole (e-–h?)
pairs effectively is the key point to achieve a good pho-
tocatalytic activity of semiconductors. Recently, noble
metal (e.g. Ag, Au, Pt, etc.) has been frequently used to
decorate photocatalysts aiming at promoting the separation
of photogenerated e-–h? pairs and hence improving their
photocatalytic performances [11–14]. It is expected that,
when photocatalysts are decorated by noble metal nano-
particles, the electrons generated in the irradiated photo-
catalysts are readily captured by noble metal nanoparticles
that act as efficient electron sinks, leaving behind the holes
on the photocatalyst surface. As a consequence, photo-
generated holes are increasingly available to participate in
photocatalytic reactions. In this work, BiFeO3 particles
with different morphologies and sizes were synthesized via
a hydrothermal route. Ag nanoparticles were deposited on
the surface of BiFeO3 particles by a chemical reduction
method to produce Ag@BiFeO3 nanocomposites. RhB was
chosen as the target pollutant to evaluate the photocatalytic
activity of prepared samples under simulated sunlight
irradiation, and the photocatalytic mechanism involved was
discussed.
2 Experimental
2.1 Synthesis of BiFeO3 particles
All raw materials and reagents used are of analytical grade
without further purification. 0.005 mol of Bi(NO3)35H2O
and 0.005 mol of Fe(NO3)39H2O were dissolved in 20 mL
of dilute nitric acid solution. Then to the mixture solution
was added 60 mL KOH solution with different concen-
trations drop by drop under magnetic stirring, and imme-
diately a dark brown suspension solution was formed. The
suspension was ultrasonically treated for 8 min and sub-
sequently stirred vigorously with a magnetic stirrer for
30 min to create a highly uniform mixture. The resulted
mixture was sealed in a Teflon-lined stainless steel auto-
clave of 100 mL capacity and submitted to hydrothermal
treatment at 200 °C. After 6 h of reaction, the autoclave
was cooled naturally to room temperature. The resulting
brown precipitate was collected and washed several times
with distilled water and absolute ethanol, and then dried in
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J Mater Sci: Mater Electron (2014) 25:2463–2469
a thermostat drying oven at 80 °C for 12 h to obtain final
BiFeO3 product. By adjusting the KOH concentration from
3 to 9 mol L-1 (M) (final concentration in autoclave), we
prepared a series of BiFeO3 samples.
2.2 Deposition of Ag on BiFeO3 particles
0.1 g of BiFeO3 particles was dispersed in 20 mL of
absolute ethyl alcohol, followed by ultrasonically treating
the suspension for 30 min. To the suspension was added
0.14 mL of 0.2 M AgNO3 solution under magnetic stirring
in ice-water bath. After adsorption for 30 min, 1.84 mL of
0.1 M NaBH4 solution was slowly dripped into the mixture
under mild stirring. Ag? ions were then reduced to form
small Ag particles onto the surface of BiFeO3 particles.
After fully depositing, the upper liquid was poured away.
The precipitate was washed several times with distilled
water, and then dried in a thermostat drying oven at 60 °C
for 4 h to obtain Ag@BiFeO3 composite particles.
2.3 Sample characterization
The phase purity of the samples was examined by means of
X-ray powder diffraction (XRD) with Cu Ka radiation. The
morphology and microstructure of the samples were
investigated by field-emission scanning electron micro-
scope (SEM) and field-emission transmission electron
microscope (TEM). The ultraviolet (UV)–visible diffuse
reflectance spectra were measured using a UV–visible
spectrophotometer with an integrating sphere attachment.
2.4 Photocatalysis evaluation
The photocatalytic activity of the samples was evaluated by
degrading RhB in aqueous solution under simulated sun-
light irradiation from a 200 W xenon lamp. The initial RhB
concentration was 5 mg L-1 and the photocatalyst loading
was 0.1 g in 200 mL of RhB solution. Before illumination,
the mixed solution was ultrasonically treated for 15 min in
the dark to make catalyst particles uniformly dispersed.
During the photocatalysis process, the water-jacketed
reactor was cooled with water-cooling system to keep the
solution at room temperature. At intervals of 1 h, 6 mL of
the reaction solution was taken and centrifuged for 10 min
at 3,000 r min-1 to remove the catalyst. The RhB con-
centration was determined by measuring the absorbance of
the solution at a fixed wavelength of 554 nm using an UV–
visible spectrophotometer. The percentage degradation is
defined as (C0 - Ct)/C0 9 100 %, where C0 and Ct are the
RhB concentrations before and after irradiation,
respectively.
J Mater Sci: Mater Electron (2014) 25:2463–2469
Scheme 1 Reaction of terephthalic acid (TPA) with OH to produce
2-hydroxyterephthalic acid (TAOH)
Fig. 1 XRD patterns of BiFeO3 samples prepared at different KOH
concentrations in precursor solution ranging from 3 to 9 M
2.5 Detection of hydroxyl (OH) radicals
Terephthalic acid (TPA) was used as a probe molecule to
examine OH radicals produced over the irradiated photo-
catalysts by simulated sunlight. TPA tends to react with OH
radicals to generate 2-hydroxyterephthalic acid (TAOH) that
is a highly fluorescent compound (Scheme 1) [15]. The pho-
toluminescence (PL) intensity of TAOH at around 429 nm is
in proportion to the amount of produced OH radicals. TPA
was dissolved in NaOH solution (1.0 mmol L-1) to make a
0.25 mmol L-1 TPA solution. 0.1 g of the catalyst was added
into 200 mL of the TPA solution. After ultrasonically treated
for 15 min in the dark, the mixed solution was irradiated by a
200 W xenon lamp (simulated sunlight). The reacted solution
was centrifuged for 10 min at 3,000 r min-1 to remove the
catalyst. The upper clear solution in the centrifuge tube was
then used for the PL measurements in a fluorescence spec-
trophotometer with the excitation wavelength of 315 nm.
3 Results and discussion
Figure 1 shows the XRD patterns of BiFeO3 samples
prepared at different KOH concentrations. Single-phase
2465
BiFeO3 samples are seen to be formed at the KOH con-
centrations ranging from 3 to 7.5 M. For these samples, all
the XRD diffraction peaks can be indexed in terms of the
rhombohedral structure of BiFeO3 with space group
R3m (PDF card no. 74-2016). However, when the KOH
concentration is raised up to 9 M, the prepared sample
presents a minor second Bi2Fe4O9 phase. This indicates
that appropriate KOH concentrations in precursor solution
are necessary in producing phase-pure BiFeO3 crystals via
the present hydrothermal synthesis route.
Figure 2 shows the SEM images of the as-prepared pure
BiFeO3 samples. The image shown in Fig. 2a reveals the
synthesis of octahedron-shaped particles with size ranging
from 500 to 600 nm when n(KOH) = 3 M. The sample
prepared at n(KOH) = 4.5 M is mainly composed of cube-
like particles in the size range of 200–500 nm (Fig. 2b).
When n(KOH) = 6 M, the resulted sample presents
irregular spherical agglomerates of 9–16 lm in size
(Fig. 2c). The higher-magnification image inserted in
Fig. 2c reveals that the agglomerates are mainly made up
of disk-like grains with diameter of 1.4–2.8 lm and
thickness of *0.2 lm. From Fig. 2d, one can see that the
sample prepared at n(KOH) = 7.5 M consists of cuboid-
shaped particles with length-to-width ratio of 1.4:1–3.5:1
and their width size distribution ranges from 80 to 280 nm.
The SEM results suggest that the precursor KOH concen-
tration has an important influence on the morphology and
size of resulted BiFeO3 particles.
The formation of BiFeO3 particles can be depicted as
three stages: (1) Bi(NO3)35H2O and Fe(NO3)39H2O were
dissolved in dilute nitric acid to form a uniform Bi3?/Fe3?
ion solution; (2) KOH was added to the solution and
reacted with Bi3?/Fe3? ions to produce amorphous
Bi(OH)3 and Fe(OH)3 precipitates; (3) Bi(OH)3 and
Fe(OH)3 reacted under the hydrothermal condition to yield
BiFeO3 particles. The ‘‘dissolution–crystallization’’ pro-
cess can be considered as a basic mechanism for the
hydrothermal formation of BiFeO3 particles [16]. Accord-
ing to this mechanism, Bi(OH)3 and Fe(OH)3 underwent an
attack of KOH to dissolve and form ion groups. BiFeO3
particles were then formed by nucleation, precipitation,
dehydration and growth, in which the crystal growth only
occurred in the region of supersaturated fluid. It is believed
that the concentration of KOH plays a critical role in the
hydrothermal formation of BiFeO3 particles. When the
KOH concentration in precursor solution was varied, the
nucleation and growth process of BiFeO3 particles could be
changed, consequently resulting in morphologically dif-
ferent products. However, when the KOH concentration
was too high, the requirement of supersaturation and stoi-
chiometry for the crystallization of BiFeO3 particles could
be locally destroyed, leading to the formation of impurity
phases (such as Bi2Fe4O9) in final product.
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Fig. 2 SEM images of BiFeO3 samples prepared at different KOH concentrations in precursor solution. a 3 M, b 4.5 M, c 6 M, and d 7.5 M

Figure 3a shows the UV–visible diffuse reflectance

Fig. 3 a UV–visible diffuse reflectance spectra of BiFeO3 samples
and b the corresponding first derivative of the diffuse reflectance
spectra
spectra of BiFeO3 samples. In order to highlight the optical
absorption features, the corresponding differential spectra
are derived and shown in Fig. 3b. It is seen that the samples
prepared at KOH concentrations of 3, 4.5, 6 and 7.5 M have
an absorption edge respectively at 564, 569, 570 and 564 nm,
which is attributed to the electron transition from valence
band to conduction band according to the theoretical results
[17]. From the absorption edge, the bandgap energy (Eg) of
the four samples is obtained to be 2.20, 2.18, 2.18 and
2.20 eV, correspondingly. The bandgap energy of the pres-
ent samples is similar to that of BiFeO3 nanoparticles pre-
pared by other methods [9, 10], but is smaller than that of
BiFeO3 films (2.5 eV) [18]. This is possibly due to the small
thickness and induced lattice expansion of the film samples.
Figure 4 shows the photocatalytic degradation of RhB
over BiFeO3 samples as a function of irradiation time (t),
along with the blank experiment result. RhB appears to be
stable without BiFeO3 photocatalyst under irradiation of
simulated sunlight, and its degradation percentage is about
5 % after 7 h of exposure. On irradiation with simulated
sunlight in the presence of BiFeO3 samples, the dye
undergoes an obvious degradation, implying that the
samples exhibit an appreciable photocatalytic activity. The
highest photocatalytic activity is observed for the sample

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Fig. 4 Photocatalytic degradation of RhB over the BiFeO3 samples
as a function of irradiation time along with the blank experiment
result
prepared at n(KOH) = 7.5 M, where the percentage deg-
radation of RhB reaches *55.1 % after irradiation for 7 h.
This is due to the fact that this sample has a relatively small
particle size. Generally, the small particle size is expected
to reduce the recombination opportunities of the photo-
generated e--h? pairs in the volume, which can effectively
move to the particle surface, and furthermore, small-sized
particles can provide more available surface active sites for
the photocatalytic reaction.
The sample prepared at n(KOH) = 7.5 M was chosen to
be decorated with Ag nanoparticles via a chemical reduc-
tion method. Figure 5 shows schematically the deposition
process of Ag nanoparticles on the surface of BiFeO3
particles. It is noted that BiFeO3 particles have an iso-
electric point at pH 5.1 [19]; that is, BiFeO3 particles bear a
negative surface charge when pH [ 5.1 and a positive
surface charge when pH \ 5.1. When AgNO3 is added to
the BiFeO3 particle suspension, the pH value of the mixture
is measured to be *6, implying that the BiFeO3 particle
surface is negatively charged. As a result, Ag? ions are
readily adsorbed onto the surface of BiFeO3 particles. By
adding the reducing agent NaBH4 thereto, the adsorbed
Ag? ions are reduced to nucleate Ag nanoparticles on the
BiFeO3 particle surface. The chemical reaction can be
represented by Eq. (1). In addition, there exists the
Fig. 5 Schematic illustration of
the deposition process of Ag
nanoparticles on the surface of
BiFeO3 particles
2467
possibility that Ag particles are nucleated in the solution,
and then they are adsorbed onto the BiFeO3 particle surface
due to their high surface energy.
2AgNO3 þ 4NaBH4 þ 10H2 O
! 2Ag þ 2NH3 þ 4NaOH þ 4BðOHÞ3 þ7H2 ð1Þ
Figure 6a, b show the TEM images of BiFeO3 particles
before and after deposition of Ag, respectively. From
Fig. 6a, one can see that bare BiFeO3 particles have a
smooth and clean surface. The image shown in Fig. 6b
reveals that Ag nanoparticles with size of 6–20 nm are
uniformly deposited on the surface of BiFeO3 crystals.
Figure 6c, d show the energy dispersive analysis of X-ray
(EDX) spectra of BiFeO3 and Ag-deposited BiFeO3 parti-
cles, respectively. Both EDX spectra present the signatures
of the constituent elements of BiFeO3 crystals. However,
additional signature from Ag element is included in the
spectrum of Fig. 6d, which gives support to the fact that,
from a chemical composition point of view, Ag nanopar-
ticles are deposited onto BiFeO3 crystals.
The photocatalytic activity of Ag@BiFeO3 composite
particles was also evaluated by degrading RhB under
simulated sunlight irradiation. The results reveal that Ag-
deposited BiFeO3 particles exhibit an enhanced photocat-
alytic activity compared to bare BiFeO3 particles. After 7 h
of photocatalysis, the percentage degradation of RhB
increases from 55.1 % for bare BiFeO3 to 79.3 % for
Ag@BiFeO3 as shown in Fig. 7.
Figure 8 shows the PL spectra of the TPA solution after
reacting for 7 h over the simulated sunlight irradiated Bi-
FeO3 and Ag@BiFeO3 photocatalysts. The blank experi-
ment result without photocatalyst is also shown in Fig. 8,
from which almost no PL signal is observed at around
429 nm. On irradiation in the presence of BiFeO3 or
Ag@BiFeO3 photocatalysts, the TPA reaction solution
shows an obvious PL signal at around 429 nm, indicating
that OH radicals are produced on the irradiated photocat-
alysts. Furthermore, when Ag@BiFeO3 is used as the
photocatalyst compared to bare BiFeO3, the PL signal
becomes more intense, implying an enhanced yield of OH
radicals on the irradiated Ag@BiFeO3 photocatalyst.
Figure 9 schematically shows the photocatalytic
mechanism of Ag@BiFeO3 photocatalyst toward the
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Fig. 6 a, b TEM images of

BiFeO3 and Ag@BiFeO3
particles, respectively. c, d EDX
spectra obtained from BiFeO3
and Ag@BiFeO3 particles,
respectively

Fig. 7 Percentage degradation of RhB after irradiation for 7 h over Fig. 8 PL spectra of the TPA solution after reacting for 7 h over the
BiFeO3 and Ag@BiFeO3 photocatalysts irradiated BiFeO3 and Ag@BiFeO3 photocatalysts by simulated
sunlight

degradation of RhB. When BiFeO3 is irradiated with light

of energy greater than its Eg, electrons are excited from the
valence band to the conduction band, leaving behind holes
in the conduction band. The photogenerated holes are
expected to react with OH- and/or H2O adsorbed on the
photocatalyst surface to generate OH radicals, which are
thought to be the dominant active species responsible for
the degradation reaction [20]. Therefore, the effective
suppression of e-–h? pair recombination and increased
availability of h? is the key point to improve the photo-
catalytic activity of the photocatalyst. It is noted that Ag
has a Fermi level of ?0.4 V versus normal hydrogen
electrode (NHE) [21], which is positive to the conduction

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Fig. 9 Schematic illustration of the photocatalytic mechanism of
Ag@BiFeO3 photocatalyst toward the degradation of RhB
band potential of BiFeO3 (?0.1 V vs. NHE) [22]. This
means that, when BiFeO3 particle surface is decorated with
Ag nanoparticles, the photogenerated electrons are ther-
modynamically favorable to transfer from the conduction
band of BiFeO3 to Ag nanoparticles. This charge transfer
process can reduce the recombination rate of e--h? pairs,
leading to an increased availability of h? for the photo-
catalytic reaction. Whereas for bare BiFeO3 particles, the
conduction band electrons tend to decay into the valence
band, resulting in a relatively high recombination rate of
e-–h? pairs. Figure 8 provides direct evidence showing an
increased yield of OH radicals on the irradiated Ag@Bi-
FeO3 compared to bare BiFeO3. As a result, decoration of
BiFeO3 with Ag nanoparticles improves the photocatalytic
activity of BiFeO3 particles.
4 Conclusions
Based on a hydrothermal route, BiFeO3 particles with dif-
ferent morphologies and sizes were synthesized by varying
the KOH concentration in precursor solution. The samples
prepared at n(KOH) = 3 and 4.5 M consist of octahedron-
shaped particles (500–600 nm) and cube-like particles
(200–500 nm), respectively. When n(KOH) = 6 M, the
resulted sample presents irregular spherical agglomerates of
9–16 lm in size which are formed from disk-like grains
(1.4–2.8 lm in diameter and 0.2 lm in thickness). The
sample prepared at n(KOH) = 7.5 M is made up of cuboid-
shaped particles with length-to-width ratio of 1.4:1–3.5:1
and their width size distribution ranges from 80 to 280 nm.
The bandgap energy of these samples is measured to be
2.18–2.20 eV. Ag-decorated BiFeO3 nanocomposites were
prepared by chemical-reduction deposition of Ag nanopar-
ticles on the surface of BiFeO3 particles. The photocatalytic
2469
experiments reveal that Ag@BiFeO3 nanocomposites exhi-
bit an enhanced photocatalytic activity for the degradation of
RhB under irradiation of simulated sunlight compared to
bare BiFeO3 particles. This can be attributed to the fact that
photogenerated electrons from BiFeO3 are effectively
transferred to Ag nanoparticles, leading to an increased
availability of holes for the photocatalytic reaction. OH
radicals are found to be produced over the simulated sun-
light irradiated BiFeO3 and Ag@BiFeO3 photocatalysts, and
furthermore an enhanced yield is observed for the latter.
Acknowledgments This work was supported by the National Nat-
ural Science Foundation of China (Grant No. 51262018) and the
Hongliu Outstanding Talents Foundation of Lanzhou University of
Technology (Grant No. J201205).
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