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Hydrothermal fabrication of monoclinic bismuth vanadate (m-BiVO 4 )

nanoparticles for photocatalytic degradation of toxic organic dyes

Research · March 2019

DOI: 10.13140/RG.2.2.19067.98088

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 Materials Science & Engineering B 242 (2019) 83–89

Contents lists available at ScienceDirect

Materials Science & Engineering B

journal homepage: www.elsevier.com/locate/mseb

Hydrothermal fabrication of monoclinic bismuth vanadate (m-BiVO4) T

nanoparticles for photocatalytic degradation of toxic organic dyes
Muhammad Munir. Sajida,c, , Nasir Amina, Naveed Akthar Shada,b, Sadaf Bashir khanc,
⁎

Yasir Javede, Zhengjun Zhangd,

⁎⁎

a
Department of Physics, Government College University, Allama Iqbal Road, Faisalabad 38000, Pakistan
b
National Institute for Biotechnology and Genetic Engineering (NIBGE), P.O. Box. 577, Jhang Road, Faisalabad, Pakistan
c
The State Key Laboratory for New Ceramics & Fine Processing, School of Materials Science & Engineering, Tsinghua University, Beijing 100084, China
d
Advanced Key Laboratory for New Ceramics, School of Materials Science & Engineering, Tsinghua University, Beijing 100084, China
e
Department of Physics, University of Agriculture, Faisalabad, Pakistan

ARTICLE INFO ABSTRACT

Keywords: Herein, we report the one pot template-free synthesis of novel monoclinic Bismuth vanadate (m-BiVO4) nano-
Bismuth vanadate particles, with highly dispersive nature and uniform size of 50–70 nm were fabricated by the facile hydrothermal
Nanoparticles method, for efficient visible light photocatalytic degradation of toxic organic dyes (Rhodamine-B and Crystal
Hydrothermal method violet). For phase, composition and chemical purity, of the as-synthesized nanoparticles were characterized by
Rhodamine-B
using X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX). To elucidate the morphology and
Crystal violet
Photocatalysis
topography, scanning electron microscopy (SEM) and transmission electron microscope (TEM) techniques were
used. For the ascription of functional groups, Fourier transforms infrared spectroscopy (FTIR) was employed.
The surface area of the as-synthesized nanoparticles was analyzed using Brunauer−Emmett−Teller (BET) and
found to be 24.946 m2/g and pore diameter 1.932 nm; m-BiVO4 nanoparticles showed enhance photocatalytic
response for the degradation for both dyes under visible light. PL study indicates the promised ability of the m-
BiVO4 nanoparticle for visible light devices.

1. Introduction technique [13], sonochemical [14], solvothermal [15], with different

interesting morphologies. Herein the BiVO4 is synthesized through fa-
Nanomaterials of the semiconductors are an important class of cile hydrothermal route; the hydrothermal method is a soft chemical
materials and are considered to have immense potential for applications procedure; it is considered to be facile, economical and en-
in the field of mechanical, magnetism, electrical, optical, electronic and vironmentally friendly benign. Moreover, dilution of precursors, reac-
catalysis as compared to their bulk counterparts owing to large surface tion temperature, pH as well as a time of reaction can be adjusted for
to volume ratio and quantum confinement characteristics [1–4]. Among amendable particle distribution, size and topography of materials par-
these semiconductors, a tertiary metal oxide, monoclinic bismuth va- ticle [16], so this route is extensively established to generate high
nadate (m-BiVO4) is an essential hetero-junction material with a narrow purity and regulated morphology materials [17].
band gap of (2.4 eV) has attracted much attention of researchers for the Organic pollutants (such as dyes) discharged from higher growth
solar energy applications such as photovoltaic, photoelectrochemical, leather; textile and food industries make great danger polluted en-
ionic conductivity and environmentally desirable “green” alternatives vironment around the globe. Rhodamine-B and crystal violet have been
for lead, non-toxic yellow pigment, chromium, excellent visible light extensively used organic materials in various industries; both these dyes
response, and photocatalytic remediation, due to its unique in- are contributing extensively to increase environmental pollution [18].
dividualities [5–8] (see Fig. 1). Nanomaterials of semiconductors for the photocatalytic degradation of
Various synthesis routes have been adopted for the preparation of harmful organic pollutants have gained much attention for wastewater
nanoscale bismuth Vanadate structures including one-pot [9], hydro- treatment. The m-BiVO4 is intensively being focused due to its char-
thermal [10], template-assisted [11], Co-precipitation [12], sol-gel acteristic degradation prospects under visible light irradiation. Various

⁎
Corresponding author: Department of Physics, Government College University, Allama Iqbal Road, Faisalabad 38000, Pakistan.
⁎⁎
Co-corresponding author.
E-mail address: [email protected] (M.M. Sajid).

https://doi.org/10.1016/j.mseb.2019.03.012
Received 22 February 2018; Received in revised form 7 March 2019; Accepted 18 March 2019
0921-5107/ © 2019 Elsevier B.V. All rights reserved.
M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Fig. 1. Schematic illustration of the hydrothermal growth of BiVO4.

novel morphologies of BiVO4 nanostructures have been reported 2. Experimental

showing excellent photocatalytic degradation of methyl orange (MO),
Congo red (CR), methylene blue dyes [19–22]. 2.1. Reagents and chemicals
In this study, we report the growth of m-BiVO4 nanoparticles about
50–70 nm using the modified hydrothermal method. The photocatalytic All the reagents were of an analytical grade in the experiment, used
activity of the as-synthesized m-BiVO4 was evaluated for degradation of deprived of any additional purification. These were purchased from
rhodamine-B (RhB) and crystal violet (CV) dyes under visible light ir- Sigma Aldrich. Ultrapure deionized water (ρ = 18 MΩ cm) from a
radiation. The m-BiVO4 nanoparticles showed excellent photocatalytic Millipore-Milli-Q system was used throughout the experiments.
activity for the degradation of both toxic dyes, referred to the high
electron-hole pair (ehp) charge separation, large active sites, increased 2.2. Synthesis of BiVO4 nanoparticles
surface area and adsorption ability of m-BiVO4 nanoparticles under
visible light. According to our knowledge, there are few reports in the In a typical synthesis, 2 mM (5 ml HNO3 solution (5 M/L)) of (Bi
literature regarding photocatalytic degradation of RhB and CV dyes (NO3)3·5H2O) was gradually added to 1 mM (20 ml) of NH4VO3 dis-
with m-BiVO4 photocatalyst. This work exposes the potential of the m- solved in 5 ml of NaOH (5 M/L) solution. Upon addition, a homogenous
BiVO4 nanoparticles for applications in environmental science and the suspension was formed which was stirred for 1 h to ensure complete
involved mechanism was probed and discussed consistently (see Tables homogenization. The pH around 8 of the system was adjusted using
1–3). 2.5 M/L ammonium hydroxide solution keep on in hydrothermal
treatment in a Teflon lined stainless steel autoclave at 180 °C for 24 h.
After the completion of hydrothermal treatment, the resulting yellowish
precipitates were collected and thoroughly washed with deionized
water (D.I.W) and absolute ethanol to ensure removal of surface-bound
impurities. The product was dried at 80 °C for 8 h before using it for the
photocatalytic degradation of RhB and CV.
Table 1
X-ray diffraction intensities and preferred growth orientation factor for BiVO4.
2.3. Characterization
HKL I Io TChkl
To investigate the crystal structure, phase purity and composition of
(1 1 2) 810 100 0.029012
(0 0 4) 257 28.4 0.673629
compounds XRD was used, X-ray Diffractometer (PANalytical Xpert)
(2 0 0) 129 18.0 0.533486 equipped with CuKα1 (λ = 1.5406 Å) X-ray source, working in 2θ
(0 2 0) 143 18.1 0.588117 (20–60) mode at room temperature. For the surface morphology, size,
(1 1 4) 120 6.9 1.294608 orientation and chemical composition of the product field emission
(0 1 5) 115 10.9 0.785376
scanning electron microscopy FE-SEM (JEOL-7500) were used. For
(−1 2 3) 88 5.3 1.235984
(2 0 4) 129 21.5 0.44664 chemical ingredients analysis, Energy Dispersive X-ray (EDX)
(0 2 4) 138 20.9 0.491517 Spectrometer characterization technique was used. Fourier transform
(2 2 0) 97 9 0.802297 infrared (FT-IR) spectrometer measurements were carried out for dif-
(−1 1 6) 166 13.4 0.922167 ferent functional groups present in the material, a Bruker Alpha spec-
(−1 2 5) 70 1.4 3.721998
trophotometer is used to record FTIR spectra. The Brunauer-
(3 1 2) 97 9.1 0.793481
(2 0 6) 125 8.4 1.107737 Emmett–Teller (BET) surface areas of the products were estimated by
using the adsorption data. Photoluminescence (PL) analysis was also

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M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Table 2
Comparison table of rate constants, “K” of BiVO4 to standard photocatalyst TiO2 for degradation of RhB and CV dyes.
Powder Rate Constant Dye Efficiency (%) Time References

−1
P-25, Degussa 0.00274 min RhB 77% 90 min [33]
P-25, Degussa – RhB 65% 120 min [34]
P-25, Degussa – RhB 60 210 min [35]
P-25, Degussa – CV 84 150 min [36]
P-25, Degussa 0.0060 min−1 CV 92% 300 min [37]
P-25, Degussa 0.003010 min−1 CV 99.99% 720 min [38]
BiVO4 0.006536 min−1 RhB 64.81% 210 min (Present study)
BiVO4 0.017259 min−1 CV 96.23% 120 min (Present study)

taken to support photocatalytic activity. Io(hkl) = Intensity of reference peak

N = Number of diffraction peaks consider in the analysis
2.4. Photocatalysis
Texture coefficient (Chkl) provides information about the preferred
To check photocatalytic responses of powdered BiVO4, samples crystal growth direction. Chkl value more than unity indicates the pre-
were illuminated under xenon lamp of an accumulative intensity of ferential growth direction for the specific plane in a diffraction pattern.
300 W to degrade CV and RhB under visible-light irradiation, the dis- In our pattern, highest Chkl value is 3.721998 for (−1 2 5) plane, and
tance between the reactor and the lamp was 20 cm. For the kinetics, the preferred growth orientation is associated to the maximum number
dyes solutions with fixed concentrations (150 ml) were prepared, and of grains along (−1 2 5) plane, which can be considered as preferential
100 mg of the as-synthesized BiVO4 nanoparticles were mixed in each growth orientation for the formation of nanoparticles as observed in the
dye solution separately. The obtained solutions were stirred vigorously SEM and TEM images.
for 30 min in the dark and subjected to illuminate under visible light Fig. 4a shows the representative micrograph of BiVO4 nanos-
irradiation at the same time. Before starting the experiment pH of the tructures obtained from scanning electron microscope (SEM) at high
compound solutions (Dye solution + nanoparticles) was maintained at magnification. SEM micrograph of the as-synthesized sample revealed
8. The final solutions were centrifuged (5000 rpm for 5 min) and ice that nanoparticles were highly dispersed with uniform size of
bath is given throughout the experiment to avoid any thermal de- 50–70 nm, which is also confirmed by TEM analysis (Fig. 4b). Sharp
gradation and to keep the temperature at 0˚C. The degradation of the morphology indicates the feasibility of formed nanostructures for the
dyes solutions was analyzed using Perkin Elmer λ 35 UV–Vis spectro- photocatalytic application. SEM micrograph at higher magnification
meter in the spectral range of 400–800 nm. The photocatalyst me- confirms the formation of nanoparticles in excessive amount. Small
chanism for the degradation of RhB and CV is indicated in Fig. 2. aggregations of nanoparticles are also observed that might because of
inter-particle interaction during the hydrothermal process. Fig. 4c re-
3. Results and discussions presents the energy dispersive X-ray spectroscopic analysis, for che-
mical composition of the as-synthesized BiVO4 indicating high crys-
Fig. 3 represents the XRD pattern of the hydrothermally synthesized tallinity of the product. Only Bi, V, and O peaks were observed, while
bismuth vanadate at 180˚C. XRD pattern corresponds to monoclinic Cu and C peaks appear due to the holding grids and carbon tape [24].
scheelite structure of BiVO4 having space group: I2/b, a = 5.193, Fig. 5 shows the FT-IR spectrum of m-BiVO4, confirming the pre-
b = 5.089, c = 11.697, γ = 90.387, well matched with the (JCPDS card sence of diverse functional groups related to BiVO4. The spectrum
No. 75-1866), that show good purity of the material. shows the absorption peak at 706.73 cm−1 corresponding to VO4. The
Texture coefficient depicts the preferential or random growth of band of V-O stretching is positioned at 519.12 cm−1, the band at
material. The texture coefficient for every hkl plane of BiVO4 has been 948.38 cm−1 is allotted to weak absorption of the Bi-O bond [25]. The
calculated from the X-rays diffraction (XRD) pattern by using the fol- symmetric and asymmetric stretching vibrations of V–O are further
lowing equation [23]. observed at 961.28 cm−1, 1004.94 cm−1 and weak absorption at
I(hkl) / Io (hkl) 477.70 cm−1 corresponding to Bi-O bond. The IR bands of very small
Texture Coefficiet = 1 intensities at 3586.76 cm−1, 3340.98 cm−1, 1634.85 cm−1 and
n (I(hkl) / Io (hkl) ) (1)
N 1137.82 cm−1 in the sample corresponding to the traces of organic
where, impurity adsorbed on the shallow of the synthesized sample using hy-
drothermal process [26].
I(hkl) = Intensity of particular XRD peak Fig. 6; indicates the nitrogen adsorption-desorption analysis using

Table 3
Comparison of Photocatalytic activity of some previously reported photocatalysts and present BiVO4 for degradation of Rhodamine-B (RhB) and Crystal violet (CV).
Materials Dye Degradation efficiency (%) Photo-degradation Time Light source References

BiVO4 nanoparticles RhB 82 180 min Visible light [39]

BiVO4 nanoparticles RhB 30 300 min Visible light [40]
BiVO4 nanoparticles RhB 64 150 min Visible light [41]
Ag2Se-G-TiO2 RhB 85.2 180 min Visible light [42]
BWO/1MG RhB 77.31 180 min Solar irradiation [43]
BiOI/GR RhB 80 240 min Visible light [44]
CdS/CdTiO3–TiO2 CV 92.59 180 min Visible light [45]
Cd-Al/C CV 52 180 min Solar irradiation [46]
Bi7O9I3/GO CV 96 1440 min Visible light [44]
m-BiVO4 nanoparticles RhB 64.81 210 min Visible light Present Work
m-BiVO4 nanoparticles CV 96.23 120 min Visible light Present Work

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M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Fig. 2. Mechanism of Photocatalysis for the degradation of RhB and CV by m- BiVO4 prepared via hydrothermal method at 180 °C.

4. Photocatalytic activity

The catalytic activity of hydrothermally prepared m-BiVO4 nano-

particles is shown in Fig. 7(a, b). Tauc’s plot method is used to analyze
the optical band gap as depicted in Fig. 7a (inset) [22,27,28], The band
gap energy for the direct transition is 2.42 eV for m-BiVO4 nano-
particles which is consistent with previous reports [27,29,30]. The ef-
fect of photocatalyst on photo-degradation rates of RhB and CV was
analyzed at different time intervals. The final solutions were examined
using Perkin Elmer λ 35 series spectrophotometer indicating the max-
imum adsorption peaks at 553 nm and 583 nm for RhB & CV organic
dyes, respectively. The efficiency of photocatalytic degradation was
measured using the following equation: (see Fig. 8).
Efficiency(%) = (C 0 - C)/C 0 × 100 (2)

where C and C0 represent the specific and initial dyes concentration for
the given time interval respectively.
After increasing the reaction time, visible photo-degradation rate of
the organic dyes is found to decrease as shown is Fig. 7(a-b). The
photocatalytic degradation efficiency is 96.23% of organic dye CV for
2 h and 64.81% of RhB dye for 3.5 h respectively. To elaborate the
Fig. 3. The XRD pattern for the as-synthesized BiVO4 nanoparticles.
reaction kinetics Pseudo first order equation was employed;

the Brunauer-Emmet-Teller (BET, ASAP-2020) to obtain the specific ln(C/Co) = Kt (3)

surface area of BiVO4, the BET surface area of bismuth Vanadate is where C represents the concentration at a specific time, Co is the con-
24.946 m2/g. It is viewed that stepwise adsorption and desorption centration at an initial time, and “k” is pseudo-first order rate constant.
hysteresis characterize by type-IV isotherm is retained, representing The values of rate constant calculated using pseudo first order equation
specific microporous material because of pore condensation having a for the degradation of both dyes using BiVO4 nanoparticles under
pore diameter of 1.932 nm. The pore size Fig. 6 (inset) shows the dis- visible light irradiation were KRhB = 0.006536 min−1 and
tribution array from 1.4020 nm to 32.1047 nm. KCV = 0.017259 min−1 respectively. The results of m-BiVO4 nano-
The BiVO4 nanoparticles relate to H2 type hysteresis loop com- particles showed admirable photocatalytic activity by maximum ad-
prising ordered pores in this type adsorption goes on homogeneously sorption amount. It indicates that catalyst has a greater affinity to
across the full volume of a porous material, but desorption takes place harvest CV as compared to RhB as shown in Fig. 7. So, when m-BiVO4
by several phenomena such as percolation and cavitation which sti- nanoparticles are subjected to visible light irradiation along with or-
mulates block and gas bubbles form in the pore internal and causes to ganic pollutants (dyes), BiVO4 nanoparticles absorb radiation, resulting
disturb porous structures. The pores are with narrow ends, bottle- in redox reaction initiation which relates to its optical band gap. As a
shaped with either end opened or one closed end. In H2 case if the pores result, electrons are endorsed from valence band (Vb) to the conduction
are small, the irregularity is comparable to pore range; this disturbs the band (Cb), the electron-hole (ehp) pair formed undergo diffusion re-
cavitation pores surrogate the pore surround which keep out abrupt sulting in redox reaction at the surface of a catalyst. The excited Elec-
from external gas because of stems undischarged to sharp pore blocking trons interact with adsorbed O2 molecules to form superoxide anion
validity. The sharp decline in desorption isotherm of BiVO4 because of radicals (O2−%); on the other hand hole in valance band oxidize OH− to
percolation and cavitation. form the hydroxyl radical species (%OH). The potential of valance band

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M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Fig. 4. (a) SEM image at magnification (X75000) (b) TEM image of BiVO4 nanoparticles (c) EDX pattern of BiVO4 synthesized by hydrothermal method at 180 °C.

Fig. 5. FT-IR spectrum of m-BiVO4 synthesised by hydrothermal method at

180 °C.
Fig. 6. Nitrogen adsorption-desorption analysis of m-BiVO4 and pore diameter
(inset) by Brunauer-Emmet-Teller.
create hydroxyl radicals ( OH) at the BiVO4 surface and potential of
%

conduction band electron adsorbed molecular oxygen leading to per-

As hydroxyl radical (%OH), is a very robust oxidizing agent which
oxide radicals [25] as revealed in equations:
hits the “OM” present at the surface of the catalyst and oxidize the dye
BiVO4 + h BiVO4 [e - + h+] (4) molecules, toxic compounds into harmless species, resulting in a pure
mineral product and CO2 is released due to the photodegradation
BiVO4 [e ] + O2 BiVO4 + O2 (5) process.

BiVO4[h+] + OH−→BiVO4+•OH (6) 5. PL study

the overall reaction is Photoluminescence (PL) spectroscopy is a versatile and widely used
BiVO4 + OH - + O2 + OM(organic matter) BiVO4 + H2 O+ CO2 to survey the separation efficiency of the charge-carrier, oxygen va-
cancy, and surface defects in semiconductors. The PL emission in-
(7)
tensities of BiVO4 nanoparticles are from the recombination of photo-

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M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Fig. 7. (a) Photocatalytic degradation of Rhodamine-B (RhB), in inset UV–visible bandgap calculated by Tauc plot method (b) Photocatalytic degradation of Crystal
Violet (CV).

excited charge-carriers. The room temperature PL emission spectrum of

pure m-BiVO4 nanoparticles is shown in Fig. 9. It can be seen that the
PL spectrum of BiVO4 nanoparticles shows strong emission peaks at
505, 510 and 542 nm in the green region of the visible light spectrum,
respectively which is inconsistent in the literature [22,31]. It is per-
ceived that this originates due to the recombination of the hole formed
in Bi 6s and O 2p and from the electron intuitive in V 3d band. There is
a blue shift in the emission bands of BiVO4 with that reported for
monoclinic BiVO4 at 550 nm, which attributed due to particle size and
shape properties of the hydrothermally synthesized BiVO4 sample [32].
It indicates the potential of the m-BiVO4 nanoparticle for visible light
devices.

6. Conclusion

In conclusion, this study explores the potential of hydrothermally

grown m-BiVO4 nanoparticles for the photocatalytic degradation of
organic dyes. The fabricated nanoparticles were elaborately char-
acterized using advanced analytical techniques including SEM, TEM,
XRD, EDX, FTIR and BET. The band gap 2.42 eV observed by UV–visible
spectra showed that m-BiVO4 nanoparticles have great potential to Fig. 9. PL emission spectra of m-BiVO4 at room temperature.
absorb light in visible light range. The PL study shows the good transfer
of photogenerated carriers in the visible range, thus leading to en-
ability of nanoparticles. The results proposed here, present a new good
hanced photocatalytic activities. The excellent size and structural uni-
photocatalytic activity of m-BiVO4 nanoparticles for visible-light-driven
formity enabled the efficient and enhanced photocatalytic degradation
photocatalysts against water remediation.
of RhB and CV under visible light irradiation. The high efficiency is
attributed to a large surface area, more active sites and light absorption

Fig. 8. (a) Degradation efficiency of BiVO4 nanoparticles and (b) Photocatalytic degradation analysis by using Pseudo first order equation.

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M.M. Sajid, et al. Materials Science & Engineering B 242 (2019) 83–89

Acknowledgements [21] C.J. Liu, Y.H. Xu, Synthesis, Characterization and Photocatalytic Activities of
Bismuth Vanadate by Facile Co-Precipitation Method, Paper presented at the
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