Facile deposition of Ag3PO4 nanoparticles on Bi2MoO6 nanoplates by microwave for highly efficient photocatalysis

Article abstract of DOI:10.1134/S003602361706016X

A simple microwave method has been successfully developed to effectively produce Ag₃PO₄/Bi₂MoO₆ nanocomposites. X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) have been employed to determine the phase and morphology of the as-produced products. The photocatalytic activities were tested through the rhodamine B (RhB) degradation under visiblelight radiation. The interaction between cubic Ag₃PO₄ nanoparticles and orthorhombic Bi₂MoO₆ nanoplates has been characterized by XRD and TEM. In this research, the as-produced heterostructure Ag₃PO₄/Bi₂MoO₆ nanocomposites display effective photogenerated charge transfer between Ag₃PO₄ and Bi₂MoO₆ which can improve charge separation. The 10.0 wt % Ag₃PO₄/Bi₂MoO₆ nanocomposites showed the highest photocatalytic performance as high as 4.36 times of the pure Bi₂MoO₆ sample.

Full text of DOI:10.1134/S003602361706016X

ISSN 0036-0236, Russian Journal of Inorganic Chemistry, 2017, Vol. 62, No. 6, pp. 836–842. © Pleiades Publishing, Ltd., 2017.
PHYSICAL METHODS
OF INVESTIGATION
Facile Deposition of Ag PO Nanoparticles on Bi MoO Nanoplates
3
4
2
6
1
by Microwave for Highly Efficient Photocatalysis
a
b,
c
Phonthep Nualkaew , Anukorn Phuruangrat *, Budsabong Kuntalue ,
d
d,
e, f
Phattranit Dumrongrojthanath , Titipun Thongtem **, and Somchai Thongtem
a
Division of Chemistry, School of Science, Walailak University, Nakhon Si Thammarat, 80161 Thailand
b
Department of Materials Science and Technology, Faculty of Science, Prince of Songkla University,
Hat Yai, Songkhla, 90112 Thailand
c
Electron Microscopy Research and Service Center, Faculty of Science, Chiang Mai University, Chiang Mai, 50200 Thailand
d
Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai, 50200 Thailand
Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai, 50200 Thailand
e
f
Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai, 50200 Thailand
*
e-mail: phuruangrat@hotmail.com
*
*e-mail: ttpthongtem@yahoo.com
Received March 18, 2016
Abstract⎯ A simple microwave method has been successfully developed to effectively produce Ag PO /Bi MoO
6
3
4
2
nanocomposites. X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission
electron microscopy (TEM) have been employed to determine the phase and morphology of the as-produced
products. The photocatalytic activities were tested through the rhodamine B (RhB) degradation under visible-
light radiation. The interaction between cubic Ag PO nanoparticles and orthorhombic Bi MoO nanoplates
3
4
2
6
has been characterized by XRD and TEM. In this research, the as-produced heterostructure Ag PO /Bi MoO
3
4
2
6
nanocomposites display effective photogenerated charge transfer between Ag PO and Bi MoO which can
3
4
2
6
improve charge separation. The 10.0 wt % Ag PO /Bi MoO nanocomposites showed the highest photocat-
3
4
2
6
alytic performance as high as 4.36 times of the pure Bi MoO sample.
2
6
DOI: 10.1134/S003602361706016X
[
10–12]. Bi MoO was reported to exhibit photocata-
In the past decades, photocatalytic semiconduct-
2 6
lytic degradation activity for 4-chlorophenol under
ing technology has attracted considerable attention
due to its great potential in water splitting and removal
of hazardous organic pollutants for wastewater treat-
visible-light radiation [10]. The photocatalytic perfor-
mance of the Bi MoO nanoplates evaluated through
2
6
the degradation of rhodamine B under Xe light irradi-
ment [1, 2]. Titanium dioxide (TiO ) is considered as
2
ation was reported to be 98.20% within 120 min [11].
the most potential material due to its chemical stabil-
ity, non-toxicity, low cost and favorable optoelec-
tronic properties [1, 3, 4]. Moreover, the application
The photocatalytic efficiency of the Bi MoO is very
2
6
low owing to the high recombination rate of electron–
hole pairs [7–9]. To improve the photocatalytic activ-
ity of visible light driven photocatalysts, the hetero-
structure photocatalyst nanomaterials were used in
order to limit the recombination rate [1, 9]. Recently, a
new type of visible-light-driven photocatalyst, Ag PO ,
of TiO is limited only under UV range (4% of sun
2
light) due to its wide band gap oxide (3.2 eV) [1, 4]. In
order to increase solar energy harvesting efficiency,
one approach is to develop new photocatalytic materi-
als of which band gap is adjusted to absorb in the visi-
ble range (about 43% of total solar energy) [1, 3, 4].
3
4
has been demonstrated to have high photooxidative
capabilities for O evolution from water, including
2
Bi MoO with a smaller band gap of 2.6 eV exhibits
2
6
organic dye decomposition under visible-light radia-
excellent photocatalytic performance under visible tion [2, 13]. Ag PO related composites have been pre-
3
4
radiation [5–9]. Moreover, Bi MoO is extremely sta- pared: Ag PO /ZnFe O [1], Ag PO /CeO [14] and
2
6
3
4
2
4
3
4
2
ble in terms of chemical, thermal and catalytic behav- Ag PO /Fe O [15].
3
4
2
3
ior [5]. Some studies have confirmed the photocata-
lytic activity of Bi MoO under visible-light radiation
In this work, Ag PO /Bi MoO nanocomposites
3
4
2
6
2
6
were prepared by a simple microwave deposition
method. Subsequently, their photocatalytic perfor-
1
The article is published in the original.
836

FACILE DEPOSITION OF Ag PO NANOPARTICLES
837
3
4
mance through the degradation of rhodamine B
RhB) under visible-light radiation was evaluated. The
photocatalytic results indicate that the heterostructure
Ag PO /Bi MoO nanocomposites can improve the
separation efficiency of charged carriers which can
lead to enhance the photocatalytic activity for RhB
degradation.
C − C
0
t
Decolorization efficiency, % =
× 100, (1)
(
C0
3
4
2
6
where C is the initial concentration of RhB and C is
0 t
the concentration of RhB after visible-light irradiation
within the elapsed time (t).
RESULTS AND DISCUSSION
EXPERIMENT
The typical XRD patterns of the obtained pure
Bi MoO and the Ag PO /Bi MoO products are
For the present research, all chemicals were analyt-
ical grade and were used without further chemical
treatment. In a typical procedure, each of 5 mmol
Bi(NO ) ⋅ 5H O and Na MoO in each 100 mL RO
2
6
3
4
2
6
shown in Fig. 1. The diffraction peaks of pure
Bi MoO and Ag PO /Bi MoO samples can be indexed
2
6
3
4
2
6
3
3
2
2
6
to orthorhombic Bi MoO (JCPDS no. 21-0102 [16]).
2
6
water was mixed together. The mixture was transferred
to a 200 mL Teflon-lined stainless steel autoclave,
tightly closed and maintained at 180°C in an electric
oven for 12 h. The obtained precipitates were washed
with distilled water and ethanol and dried at 80°C for
They should be noted that the (210) main characteristic
diffraction peak of cubic Ag PO (JCPDS no. 06-0505
3
4
[
16]) at 2θ = 33.26° overlapped the (002) peak of ort-
horhombic Bi MoO phase. Thus, the Ag PO phase
2
6
3
4
24 h for further characterization.
was unable to be detected by this XRD analysis although
the sample was composed of 10.0 wt % Ag PO .
3
4
To synthesize different contents of Ag PO
3
4
nanoparticles deposited on the Bi MoO samples,
The morphology and microstructure of pure
.0–10.0 wt % of AgNO and Na PO of each 1.0 g Bi MoO and Ag PO /Bi MoO samples were investi-
2
6
0
3
3
4
2
6
3
4
2
6
Bi MoO sample were dissolved in 100 mL RO water. gated by SEM. Fig. 2a shows that the obtained Bi MoO
6
2
6
2
They were heated at 180 W microwave for 15 min. Subse- appeared as nanoplates with edge of approximately 1 μm
quently, the products were separated by filtering, washed long. The 5.0 wt % and 10.0 wt % Ag PO /Bi MoO
6
3
4
2
with absolute ethanol and dried at 80°C for 24 h.
composites (Figs. 2b, 2c) show Ag PO nanoparticles
3 4
deposited on the surface of Bi MoO after being
Phase of the as-synthesized products was investigated
by an X-ray diffractometer (XRD, Philips X’Pert MPD)
2
6
heated by microwave, and formed Ag PO /Bi MoO
6
3
4
2
−
1
nanocomposites. At high-magnification of 10.0 wt %
Ag PO /Bi MoO (Fig. 2d), the size of cubic Ag PO
4
with CuK radiation operating at 30 kV and 0.02° ⋅ s
α
o
scanning rate in the 2θ range of 15°–60 . Morphology
and microstructure of the products were character-
ized by a field emission scanning electron micro-
scope (FE-SEM, JEOL JSM-6335F) equipped with
3
4
2
6
3
nanoparticles on the Bi MoO nanoplates was around
2
6
2
0 nm. The elemental mapping of the 10.0 wt %
Ag PO /Bi MoO nanocomposites was detected by
3
4
2
6
an Oxford instruments INCA energy dispersive X-ray EDX spectroscopy, as the results shown in Fig. 3. In
(
EDX) spectrometer operating at 35 kV, including a this research, Ag, P, Bi, Mo and O were detected, indi-
transmission electron microscope (TEM, JEOL cating that the composites were mainly composed of
JEM-2010) operated at 200 kV. Nitrogen adsorp- the elemental constituents. The EDX mapping con-
tion/desorption isotherms were measured at 80°C firms that the Ag PO nanoparticles were uniformly
3
4
using a Quantachrome Autosorb 1 MP automated gas distributed across the Bi MoO nanoplates.
2
6
adsorption system and calculated on the basis of
Brunauer–Emmett–Teller (BET) surface analysis.
The photocatalytic activities of the products were
evaluated via the photodegradation of rhodamine B
In addition, the morphologies of Bi MoO and
2
6
Ag PO /Bi MoO samples were investigated by TEM
3
4
2
6
as shown in Fig. 4. The TEM image reveals the
Bi MoO nanoplates with the edge of ca 200–400 nm.
2
6
(
RhB) in aqueous solutions under visible-light radia-
The SAED pattern of a single Bi MoO nanoplate
2
6
tion. For each experiment, 50 mg photocatalyst was
−5
shows spots of electron diffraction pattern, implying
the presence of single crystalline nanoplate. The pat-
tern can be indexed to (060), (062) and (002) planes
with zone axis along the [100] direction. For the
put in 200 ml of 1 × 10 M RhB aqueous solution.
Before illumination, the suspensions were stirred in
the dark to obtain saturated adsorption of RhB on the
surface of catalyst for 30 min. Then the visible light
was turned on. During testing, each 5 mL of the sus-
pension solution was sampled for every 30 min inter-
val. The sampled solutions were spun to precipitate the
suspensions. The RhB concentration was determined
by a UV-visible spectrometer (Perkin Elmer, Lambda
1
0.0 wt % Ag PO /Bi MoO nanocomposites, the
3 4 2 6
small Ag PO nanoparticles with the size of about 10–
3
4
1
5 nm were firmly bound on the surface of Bi MoO
2 6
nanoplates. They enhanced electron transfer between
Ag PO nanoparticles and Bi MoO nanoplates, as
3
4
2
6
2
5 UV-VIS spectrometer) and decolorization effi- well as improving the photocatalytic efficiency.
ciency was calculated by the equation
HRTEM image of 10.0 wt % Ag PO /Bi MoO nano-
3
4
2
6
RUSSIAN JOURNAL OF INORGANIC CHEMISTRY Vol. 62 No. 6 2017

8
38
PHONTHEP NUALKAEW et al.
1
0% Ag PO /Bi MoO
3 4 2 6
5
% Ag PO /Bi MoO
3
4
2
6
Bi MoO
2
6
15
20
25
30
35
2
40
θ, deg
45
50
55
60
Fig. 1. XRD patterns of Bi MoO , 5.0 wt % Ag PO /Bi MoO and 10.0 wt % Ag PO /Bi MoO samples.
2
6
3
4
2
6
3
4
2
6
composites exhibits lattice fringe with d = 0.27 nm, moted electron transfer between Ag PO nanoparti-
3
4
corresponding to the (210) plane of cubic Ag PO .
cles and Bi MoO nanoplates.
2 6
3
4
To evaluate the photocatalytic activity of the as-
The RhB photodegradation was investigated by
obtained photocatalysts, RhB was used as a target sub- Bi MoO containing different contents of Ag PO
4
2
6
3
stance to test the photocatalytic performance under under visible-light radiation. The absorbency at the
visible-light radiation (λ ≥ 420 nm). Figure 5a,b shows vertex of the RhB peak (554 nm) for different lengths
the temporal evolution of absorption spectra of RhB of time was plotted, as the results shown in Fig. 5c.
dye degradation by Bi MoO and 10.0 wt % Clearly, the photocatalytic activity increased with the
2
6
Ag PO /Bi MoO under visible illumination within increase of Ag PO content. Within 240 min, the
3
4
2
6
3
4
different lengths of irradiation time. Obviously, the decolorization efficiency of RhB by Bi MoO and
2
6
decrease of RhB concentration with a major absorp- 10.0 wt % Ag PO /Bi MoO was around 22.38 and
3
4
2
6
tion peak at around 554 nm by 10.0 wt % 97.54%, respectively. The decolorization efficiency of
Ag PO /Bi MoO is faster than that by Bi MoO . The RhB by 10.0 wt % Ag PO /Bi MoO is 4.36 times of
3
4
2
6
2
6
3
4
2
6
RhB with a major absorption peak at around 554 nm that by Bi MoO . In addition, the photocatalytic
2
6
by 10.0 wt % Ag PO /Bi MoO gradually decreased
3
4
2
6
activity is influenced by the BET surface area: the sur-
2
towards zero within 240 min irradiation. The absorp-
tion peak shifted from 554 nm to 498 nm caused by the
change of RhB molecules in sequence: Rhodamine B
face area of Bi MoO (14.82 m /g) is almost the same
2
6
2
as that of 10.0 wt % Ag PO /Bi MoO (10.32 m /g).
3
4
2
6
Thus, the content of Ag PO is an important parame-
3
4
(
554 nm) to N,N,N′-Triethyl rhodamine (540 nm),
ter to play a significant role in the photocatalytic reac-
tion rate. Two main processes are possible. (1) Ag PO
N,N′-Diethyl rhodamine (522 nm), N-Ethyl
3
4
Rhodamine (510 nm) and Rhodamine (498 nm) [17,
nanoparticles have photocatalytic activity [13] which
can improve the photodegradation rate. (2) Ag PO
1
8]. The 50% Ag PO loaded Bi MoO spheres were
3 4 2 6
3
4
6
reported to exhibit the highest photocatalytic activity
in the decolorization of RhB [19]. For the present
work, the 10.0 wt % Ag PO /Bi MoO showed the
nanoparticles are effectively bound on Bi MoO
2
nanoplates, and the Ag PO /Bi MoO composites can
3
4
2
6
3
4
2
6
enhance photodegradation rate [1, 4].
highest photocatalytic activity in the decolorization of
RhB due to the uniform distribution of Ag PO
3
4
In order to investigate the kinetics of photocatalytic
nanoparticles on Bi MoO nanoplates which pro- degradation, the Langmuir–Hinshelwood equation as
2
6
RUSSIAN JOURNAL OF INORGANIC CHEMISTRY
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2017

FACILE DEPOSITION OF Ag PO NANOPARTICLES
839
3
4
1
μm
1 μm
(a)
(b)
1
μm
100 nm
(c)
(d)
Fig. 2. SEM images of (a) Bi MoO , (b) 5.0 wt % Ag PO /Bi MoO and (c, d) 10.0 wt % Ag PO /Bi MoO .
2
6
3
4
2
6
3
4
2
6
(a)
(b)
(c)
WD 15.2 mm ×20.000
1 μm
(d)
(e)
(f)
Fig. 3. (a) SEM image and (b–f) EDX mapping of Ag, P, Bi, Mo and O of 10.0 wt % Ag PO /Bi MoO nanocomposites, respec-
3
4
2
6
tively.
a pseudo-first-order kinetics is usually used to respectively [20–22]. If the initial concentration is suf-
describe the reaction rate by the following
ficiently small, simplification of this kinetic equation
into a pseudo first-order equation is frequently
(2) employed and given by the following
dCt
dt
k C
TC t
−
= K
,
1 + k C
TC
0
⎛
C ⎞
0
⎟
where K and k are the Langmuir Hinshelwood
TC
ln
= k t ,
(3)
⎜
app
adsorption coefficient and reaction rate constant,
⎝Ct ⎠
RUSSIAN JOURNAL OF INORGANIC CHEMISTRY Vol. 62 No. 6 2017

8
40
PHONTHEP NUALKAEW et al.
(062)
(060)
(002)
200 nm
(a)
(b)
50 nm
10 nm
(c)
(d)
Fig. 4. (a) TEM image and (b) SAED pattern of pure Bi MoO and (c, d) HRTEM images of 10.0 wt % Ag PO /Bi MoO nano-
2
6
3
4
2
6
composites.
where k = Kk is the pseudo-first-order rate con- valence band of Bi MoO (+2.71 eV vs NHE) [23]
app
TC
2
6
−
1
stant (min ) [10, 12, 20]. Figure 5d describes the liner
migrate into the valence band of Ag PO (+2.63 eV vs
NHE) [24]. The holes were scavenged by H O to form
OH on the Ag PO surface [13] because E of
3
4
relationship between ln(C /C ) and reaction time t,
0
t
2
where the slope of the linear line is the pseudo-first-
order apparent rate constant. The apparent rate con-
stant for the degradation of RhB by 10.0 wt % Ag
•
3
4
VB
•
PO is more positive than the E° (OH /H O) =
3
4
2
−
1
Ag PO /Bi MoO is 0.0125 min , which is 14.29 times +2.27 eV [24]. These active species decomposed
3
4
2
6
−
4
−1
of that by Bi MoO (8.75 × 10 min ). The increase
2
6
rhodamine B into the final or other intermediate
products.
of the k is the result of the high migration efficiency
app
of photoinduced electrons to enhance photocatalytic
activity of Ag PO /Bi MoO .
3
4
2
6
CONCLUSIONS
Based on the above, the Ag PO /Bi MoO nano-
3
4
2
6
composites possess excellent photocatalytic activity
for the degradation of RhB. Under visible light,
Ag PO and Bi MoO were excited to produce photo-
In summary, visible-light-response Ag PO /Bi MoO
6
3
4
2
nanocomposites were produced by a microwave radia-
3
4
2
6
tion method. The experimental results showed that the
generated electrons and holes. The photogenerated
extra effect of Ag PO and Bi MoO was very important
electrons in conduction band of Bi MoO (−0.32 eV vs
3
4
2
6
2
6
NHE) [23] migrate to the conduction band of Ag PO
to enhance the photoactivity of Ag PO /Bi MoO . The
3 4 2 6
3
4
(
+0.27 eV vs NHE) [24] at the Ag PO /Bi MoO
3 4 2
interfaces of the two materials can slow down the high
6
interface. The photogenerated electrons in the con- electron–hole recombination rate and can speed up
duction band of Ag PO could be trapped by the the highly efficient photocatalysis. Thus the hybrid
3
4
adsorbed O to produce H O and further decomposed composites are the promising materials for the envi-
2
2
2
•
to OH radicals [25]. Concurrently, the holes in ronmental purification.
RUSSIAN JOURNAL OF INORGANIC CHEMISTRY
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FACILE DEPOSITION OF Ag PO NANOPARTICLES
841
3
4
(a)
(b)
0
min
0 min
30 min
3
6
9
0 min
0 min
0 min
60 min
90 min
120 min
150 min
180 min
210 min
240 min
1
20 min
1
50 min
80 min
10 min
40 min
1
2
2
4
00
450
500
550
600
650
700 400
4
450
500
550
600
650
700
Wavelength, nm
Wavelength, nm
0
(c)
(d)
2
4
6
8
0
0
0
0
Bi MoO
2
6
3
2
1
0
2
.5% Ag PO /Bi MoO
3 4 2 6
5
% Ag PO /Bi MoO
6
3
4
2
10% Ag PO /Bi MoO
3
4
2
6
Bi MoO
2
6
2.5% Ag PO /Bi MoO
3
4
2
6
5
1
% Ag PO /Bi MoO
3 4 2 6
0% Ag PO /Bi MoO
3 4 2 6
100
0
40
80
120
160
200
240
0
40
80
120
160
200
240
Time, min
Time, min
Fig. 5. (a, b) UV-visible absorption of RhB in the solution containing Bi MoO and 10.0 wt % Ag PO /Bi MoO nanophoto-
2
6
3
4
2
6
catalysts under visible-light radiation within 240 min. (c) Decolorization efficiency and (d) first-order plot of the photocatalytic
activity of Bi MoO , 2.5 wt % Ag PO /Bi MoO , 5.0 wt % Ag PO /Bi MoO and 10.0 wt % Ag PO /Bi MoO nanophotocat-
2
6
3
4
2
6
3
4
2
6
3
4
2
6
alysts under visible-light radiation within 240 min.
ACKNOWLEDGMENTS
6. X. Zhao, T. Xu, W. Yao, et al., Appl. Surf. Sci. 255, 8036
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(
We are extremely grateful to the Faculty of Science
Research Fund, Faulty of Science, Prince of Songkla
University, Thailand for providing financial support,
and Chiang Mai University, Thailand for providing
financial support through the Center of Excellence in
Materials Science.
7
8
9
(
(
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0. V. Umaoathy, A. Manikandan, S. Arulantony, et al.,
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