A facile synthesis of a highly efficient β-Bi2O3/Bi2O2CO3heterojunction with enhanced photocatalytic NO oxidation under visible light

Article abstract of DOI:10.1039/d0nj01325k

The construction of a β-Bi2O3/Bi2O2CO3 heterojunction is an effective approach to separate the photogenerated charge carriers and to improve the photocatalytic performance of the semiconductor photocatalysts. In this study, a composite nanosheet of β-Bi2O3/Bi2O2CO3 was fabricated via an in situ annealing of Bi2O2CO3 at 380 °C. The composite showed an excellent adsorption toward NO and an enhanced photocatalytic efficiency over NO oxidation from 5.7 v/v% (bare Bi2O2CO3) to 32.5 v/v% (β-Bi2O3/Bi2O2CO3). Furthermore, the presence of the β-Bi2O3/Bi2O2CO3 heterojunction promoted the formation of additional O2-, and then improved the NO oxidation activity and safety of BOC in conjunction with OH. This journal is

Full text of DOI:10.1039/d0nj01325k

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A facile synthesis of a highly efficient b-Bi O /
2
3
Bi O CO heterojunction with enhanced
2
2
3
Cite this:DOI: 10.1039/d0nj01325k
photocatalytic NO oxidation under visible light†
Yaru Hao, * Zhaoqi Deng, Ziquan Zhao and Xijia Song
The construction of a b-Bi
photogenerated charge carriers and to improve the photocatalytic performance of the semiconductor
photocatalysts. In this study, a composite nanosheet of b-Bi /Bi CO was fabricated via an in situ
annealing of Bi CO at 380 1C. The composite showed an excellent adsorption toward NO and an
enhanced photocatalytic efficiency over NO oxidation from 5.7 v/v% (bare Bi CO ) to 32.5 v/v%
b-Bi /Bi CO ). Furthermore, the presence of the b-Bi /Bi CO heterojunction promoted the
2 3 2 2 3
O /Bi O CO heterojunction is an effective approach to separate the
2
O
3
O
2 2
3
Received 17th March 2020,
Accepted 26th May 2020
2
O
2
3
2
O
2
3
(
O
2 3
2
O
2
3
O
2 3
2
O
2
3
DOI: 10.1039/d0nj01325k
ꢀ
2À
formation of additional
O
, and then improved the NO oxidation activity and safety of BOC in
ꢀ
rsc.li/njc
conjunction with OH.
process and fast recombination of the photogenerated electrons
1
. Introduction
7
,19
and holes.
Therefore, numerous related studies have been
In the past decades, the quest for the efficient use of solar energy conducted to solve these problems, including the band structure
has been motivated by successfully employing the artificial anatase modification, the crystal facet control and the heterojunction
1
–3
20–24
TiO
2
photonic crystals for the splitting of water. To take full construction.
In particular, some studies demonstrated that Bi
the development of varied photocatalysts. Among the varied converted to a metastable b-Bi via an annealing process.
photocatalysts, bismuth photocatalysts (e.g., Bi , BiO CO , BiVO crystal structure of b-Bi is similar to that of Bi CO , which is
and BiOX, X = Cl, Br, and I) with their nontoxic properties and attributed to the same atomic arrangement in their Bi
tunable electronic structures have been one of the most promising Therefore, the integration of these two phases is expected to form a
advantage of the solar energy, most efforts have been focused on
2 2 3
O CO can be
4
,5
25–27
2
O
3
The
2
O
3
2
3
4
,
2
O
3
2
O
2
3
2
+
28
2
O
2
layers.
6
–14
material series.
been widely explored during the past year
of hybridized valence band (VB) by the Bi 6s and 2p levels, which and less negative CB of the component semiconductors, respec-
could produce increased mobility of photogenerated holes during tively. For example, a b-Bi /Bi CO composite exhibited a
photocatalysis. However, Bi CO has a wide band gap (ca. 3.4 eV), much higher photodegradation efficiency toward MB than bare
indicating that it can only be excited by UV light. To extend the Bi
response of Bi CO to the visible light region, the construction of carrier migration cannot include both the oxidizing power of
a heterojunction of Bi O CO with another narrow band gap holes and the reducing power of electrons simultaneously. In
Bi O CO , a Bi(III)-based semiconductor, has p–n junction, in which the charge carrier separation is achieved
2 2 3
1
5–17
due to the formation through the migration of holes and electrons to the less positive VB
2
O
3
2
O
2
3
2
O
2
3
8
29
2
O
2
CO
3
and b-Bi
2
O
3
.
Unfortunately, such type of charge
2
O
2
3
2
2
3
semiconductor system has become an efficient option. It is worth contrast, the proposed Z-scheme heterojunction could avoid
noting that tetragonal-Bi(III) oxide (b-Bi O ) with a narrow band gap this shortcoming, in which the migration of electrons is from
2
3
3
of ca. 2.61 eV among the other Bi(III)-based semiconductors has the less negative CB of one semiconductor such as WO to the
10,18
30
been intensively studied for various applications.
valence band (VB) of b-Bi is sufficiently positive, it has been
barely individually used in previous studies because of its less Z-scheme heterojunction of b-Bi
negative conduction band (CB), instability in the reaction treatment. The photocatalytic activity of the b-Bi
Although the less positive VB of the other semiconductor g-C
In this study, we reported the facile fabrication of a layered
/Bi CO via a thermal
/Bi CO
3
3 4
N .
2 3
O
2
O
3
2
O
2
3
2
O
3
2
O
2
composite was evaluated by the photocatalytic oxidation of
ppb-level NO under the irradiation of visible light. Moreover,
the photogenerated superoxide radicals among the b-Bi O /
University of Electronic Science and Technology of China, Zhongshan Institute,
No. 1 Xueyuan Road, Zhongshan 528402, China. E-mail: 165689908@qq.com;
Tel: +0760 88227202
2
3
2 2 3
Bi O CO composite promotes fast migration owing to the
Z-scheme mechanism, which is beneficial for obtaining
†
Electronic supplementary information (ESI) available. See DOI: 10.1039/
d0nj01325k
enhanced photocatalytic activity.
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2. Experimental
2
.1. Preparation of samples
Synthesis. All of the chemicals used in this study were of
analytical grade and obtained from Shanghai Chemical. Bi CO
BOC) samples were synthesized by modifying a reported method.
In a typical synthesis, 4.85 g of Bi(NO O was dissolved in 10
Á5H
mL of 1 M HNO aqueous solution and further stirred for 40 min at
2
O
2
3
15
(
3
)
3
2
3
room temperature to form a clear solution (denoted as solution A).
Moreover, 1.0 g of cetyltrimethylammonium bromide (CTAB) and
8
.45 g of Na CO Á10H O were added to 90 mL of distilled water
2
3
2
(denoted as solution B). Then, solution A was dropped into solution
B under constant stirring. After 10 min of stirring, the resulting
Fig. 1 PXRD patterns of the as-prepared Bi
2
O
2
CO
3
and the samples after
white precipitate was filtered, washed with ultrapure water and annealing at different temperatures.
ethanol for five times and dried at 60 1C for 12 h to obtain BOC
samples with no further treatment. Finally, the BOC precursors
simultaneously, which suggested the formation of the b-Bi
2 3
O /
were calcined in the temperature range from 350 1C to 420 1C for
h under atmospheric conditions to obtain different samples. The
Bi CO composites. In line with the PXRD patterns, the UV-vis
2
O
2
3
4
absorption edge of these samples also shifted from 356 to 507 nm
obtained samples were denoted as BOC-350, BOC-380, BOC-400
and BOC-420, corresponding to the temperatures 350 1C, 380 1C,
with an increase in the temperature (Fig. 2). The band gap (E ) was
g
evaluated using the following equation E = 1240/l. Therefore, the
400 1C and 420 1C, respectively.
g
band gaps (E
were approximately determined as 3.25, 2.57, 2.52, 2.46 and
.20 eV, respectively. The absorption band edge of BOC-380 was
g
) of BOC, BOC-350, BOC-380, BOC-400 and BOC-420
2.2 Characterization
2
Powder X-ray diffraction (PXRD) was conducted on a PANalytical
X’pert diffractometer operated at 40 kV and 40 mA using a Cu Ka
radiation. Diffuse reflectance spectra (DRS) were recorded on a
Shimadzu UV-2600 spectrophotometer equipped with an inte-
significantly smaller than that of BOC, which suggested that
BOC-380 facilitated the visible light harvesting.
The photocatalytic activities of these samples were evaluated
by the photocatalytic oxidation of ppb-level NO in air under
visible light irradiation (l 4 420 nm). In Fig. S1 of the ESI,† it is
observed that NO is very stable and cannot be photolyzed under
visible light irradiation in the absence of photocatalysts. Before
irradiation, all the catalysts were exposed to the starting NO gas
until reaching an adsorption–desorption equilibrium under
experimental conditions. The photooxidation of NO for BOC-380
could reach as high as 32.5% v/v in 7.5 min (Fig. 3a), while the
removal ratio of NO over BOC was quite low (5.7% v/v).
A conventional TiO2 (P25) photocatalyst exhibited almost no
photocatalytic NO oxidation activity under the same condition
photocatalytic activity as shown in Fig. S2 (ESI†), which is due
to a wide band gap. However, the photooxidative ability of NO
on BOC-350, BOC-400 and BOC-420 was not in good agreement
with BOC-380. Therefore, the optimum proportion of the
catalyst concentration between Bi O CO and b-Bi O3 may
grating sphere using BaSO as the reflectance standard sample.
4
Scanning electron microscopy (SEM) was performed on a Hitachi
S-4800 microscope. TEM images were obtained on an FEI Tecnai
G2 20 microscope at 200 kV. X-ray photoelectron spectroscopy
(XPS) measurements were conducted on a Thermo ESCALAB
250Xi with Al Ka emission at 1486.6 eV. All binding energies
were referenced to the C 1s peak at 284.8 eV. A JE-SFA200
spectrometer was used to detect the in situ electron spin
resonance (ESR) signals of the samples using DMPO as the
capturing reagent. The photocatalytic measurements of NO
oxidation were completed using a self-built photocatalytic
evaluation device. The removal ratio (Z) of NO was calculated
as Z (%) = (1 À C/C
0
) Â 100%, where C and C
0
are the
concentrations of NO in the outlet stream and the feeding stream,
respectively. The detailed measurements are shown in the ESI.†
2
2
3
2
3. Results and discussion
The PXRD spectra of the as-fabricated samples are shown in Fig. 1.
In the PXRD spectra, the diffraction peaks of the as-prepared BOC
can be assigned to the tetragonal Bi
The signal of b-Bi appeared with the obtained BOC, which was
annealed under atmospheric conditions at temperatures of 350,
80, 400 and 420 1C. When the annealing temperature reached
about 380 1C, typical peaks appeared at around 27.91, 31.81 and
2 2 3
O CO (JCPDS no. 41-1488).
2 3
O
3
3
2.71, which corresponded well with the values from the b-Bi O3
2
standard card (JCPDS no. 27-0050). With the further increase in
Fig. 2 (a) UV-vis diffuse reflectance spectra and (b) plots of transformed
Kubelka–Munk function versus the energy of absorbed light for as-
2 2 3
temperature, the diffraction peaks of Bi O CO in the samples
2 3
gradually decreased, while the peaks of the b-Bi O
phase enhanced prepared samples under annealing at different temperatures.
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2
À
Consequently, the electronic densities of C in the CO
3
layers were
also affected by the b-Bi formed. The peak at 530.9 eV can be
2 3
O
ascribed to the oxygen of the C–O bond, and the dominant 529.6 eV
peak of O 1s characterized by the Bi–O bonds in Bi O CO shifted
2
2
3
32
to 529.9 eV, belonging to b-Bi O (Fig. 5b). The other peaks are
2
3
33
from adsorbed H
2
O on the surface. The two strong peaks at
1
58.9 and 164.2 eV are assigned to Bi 4f7/2 and Bi 4f5/2, which
+
11
correspond to Bi
Fig. 3 Photocatalytic oxidation of NO over the as-prepared samples of same as those obtained from pure b-Bi
BOC, BOC-350, BOC-380, BOC-400 and BOC-420 under visible light
irradiation (l 420 nm): (a) photocatalytic removal ratio of NO;
b) generation of NO
3
(Fig. 5c). These values are not exactly the
or Bi CO after the
2 3
annealing of BiO CO at 380 1C, which indicates that an interfacial
2
O
3
2
O
2
3
4
structure is formed and the local environment and electron density
of the elements changed to some extent. These results were well
agreed with the XRD analysis. The EVB of Bi O C and BOC-380 are
(
2
.
2
2 3
effectively separate and transfer the photogenerated charge estimated to be 1.77 and 2.13 eV, respectively, which is observed
ꢀ
À
ꢀ
carriers for the production of O and OH reactive species.
from the VB-XPS spectra (Fig. 5d). In addition, the ECB of pure
The morphology and the microstructure of these samples Bi CO could be constructed using the following empirical
were further investigated by the SEM and TEM observations. formulae: ECB = EVB À E . According to the above formulae, the
The SEM images of the samples prepared, BOC and BOC-380,
VB and ECB values of pure Bi CO were calculated to be 1.77 and
are shown in Fig. 4a and b. The prepared BOC constitutes À1.48 eV, respectively. Zhou also reported that the EVB value of pure
large amounts of loose microspheres. Evidently, the image of Bi CO was 1.76 eV, which was obtained from the ultraviolet
BOC-380 appeared to be irregular nanosheets due to the release photoelectron spectrum. The EVB by XPS measurement and ECB
of H O and CO gas during decomposition. These results values of pure b-Bi were calculated to be 2.59 and 0.31 eV,
2
2
O
2
3
g
E
2
O
2
3
O
2
2
3
3
4
2 3
O
2
2
10
suggested that the Bi O CO nanosheets gradually transformed respectively.
2
2
3
to b-Bi O . The HRTEM image of BOC showed a clear lattice
The spin-resonance technique (ESR) was further employed
2
3
fringe with an interplanar lattice spacing of 0.274 nm and an to detect the active species generated during the photocatalytic
angle of 901 (Fig. 4c), which corresponded with the (110) plane NO oxidation of BOC and BOC-380 (Fig. 6a and b). Some
ꢀ
of the tetragonal Bi
2
O
2
CO
3
. It clearly showed two different negligible signals corresponding to DMPO– OH of BOC and
fringes with spacings of 0.274 and 0.323 nm (Fig. 4d), corres- BOC-380 under the same conditions of light irradiation can be
ponding to the (110) lattice plane of Bi CO
and (201) plane detected in Fig. 6a. As shown in Fig. 6b, the characteristic peaks
of the tetragonal b-Bi O . These results further confirmed that of DMPO– O
2
O
2
3
ꢀ
À
2
3
2
for BOC are very weak; however, 6 strong signals
in BOC-380 are detected after 10 min under visible light
b-Bi O nanosheets were formed in situ on Bi O CO .
2
3
2
2
3
ꢀ
À
The survey and the high-resolution XPS spectra of BOC and condition. These results confirmed that O
2
is the dominant
BOC-380 are shown in Fig. 5. It is observed that the peak of C 1s active species in the photocatalytic degradation process. The
at 284.8 eV can be ascribed to the adventitious carbon species activity of the photocatalyst is related to the absorption of light,
31
from the XPS measurements, which remained unchanged, the absorption intensity, and the separation of photogenerated
whereas the peaks at 288.8 and 285.3 eV belonging to the carbonate electrons and holes. Photoluminescence (PL) is a typical tech-
in BOC shifted up to 288.9 and 287.3 eV in BOC-380 (Fig. 5a). nique for studying the photon-generated carrier properties of
Fig. 4 SEM (a and b) and HRTEM (c and d) images of BOC and BOC-380,
Fig. 5 XPS spectra of BOC and BOC-380: (a) C 1s, (b) O 1s, (c) Bi 4f, and
respectively.
(d) valence band.
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Fig. 7 Possible photocatalytic oxidation mechanism of NO on BOC-380.
(
a) Before connection. (b) After connection.
can effectively separate the electron–hole pairs, which is called
À
the Z-scheme heterojunction. The separated e on the CB of
ꢀ
Fig. 6 ESR spectra of (a) hydroxyl radicals ( OH) and (b) superoxide
+
Bi O CO and h on the VB of b-Bi O then freely migrated
ꢀ
À
2
2
3
2 3
radicals ( O ), and PL spectra of BOC and BOC-380 (c).
2
toward the surface to react with the adsorbed reactants, leading
to an enhanced photocatalytic activity in the composites. In
order to understand the photocatalytic process, in situ FTIR
was subsequently carried out to intuitively reveal the conversion
pathways for the photocatalytic NO oxidation (Fig. S3, ESI†). Two
the semiconductor materials. Studies have shown that the
fluorescence intensity is related to the recombination rate of
À
+ 13,14
electrons (e ) and holes (h ).
For this reason, the PL spectra
À1
intensive broad bands at 1247 and 1189 cm could be evidently
of BOC, BOC-380 and BOC-420 are measured under the excita-
tion of a 367 nm laser (Fig. 6c). In general, the charge carrier
migration followed the p–n heterojunction pathway, that is,
observed in the NO adsorption process on b-Bi O /Bi O CO
3
2
+
3
37
2
2
(
Fig. S3a, ESI†), which could be assigned to NO . The weak
À1
À 38
band at 1094 cm was observed for NO .
3
After light on, the
À
2
bands at 1290 and 1056 cm gradually strengthened, which
electrons from the CB of BOC migrated to the CB of b-Bi
2
O
3
À1
+
NO
had formed by the oxidation of NO with O
bands at 817, 1020, 1056 and 1093 cm assigned to NO
transformed from NO
attributed to the OH and NO
and h from the VB of b-Bi O to the VB of Bi O CO , resulting
2
3
2
2
3
ꢀ
À1
À
(reaction (3)). The
in the PL intensity of BOC lower than that of BOC-380 and
BOC-420. Nevertheless, the peak intensity of BOC-380 was
obviously stronger than that of BOC and BOC-420, indicating
stronger charge carrier recombination in BOC-380. According
2
À
3
was
À
À
37–39
2
species (Fig. 3Sb, ESI†).
This could be
ꢀ
À
2
participating in the photo-
3
5,36
catalytic oxidation (reaction (5)). During the photocatalytic
to the similar results from previous studies,
the Z-scheme
À1
reaction, new peak bands at 873 cm assigned to the adsorption
pathway was the only explicable reason for the increase in the
40
+
À
of NO also appeared. From the comparative investigations
above, the photocatalytic removal of NO over BOC-380 may
involve the following reactions:
PL intensity. This process could consume h and e from the
VB of Bi O CO and the CB of b-Bi O , while preventing
2
2
3
2 3
À
+
the recombination of e and h from the CB of Bi O CO and
2
2
3
the VB of b-Bi
2
O
3
.
À
+
hn + BOC-380 - e + h
(1)
(2)
(3)
(4)
(5)
Based on the discussion of the abovementioned experi-
mental results, we presented the photocatalytic mechanism of
the NO removal by a composite catalyst sample under visible
À
ꢀ
2 2
+ O - O
e
ꢀ
2À
+ NO - 2NO
O
2
light. It is known that b-Bi
Bi CO is an n-type semiconductor. Therefore, after their
contact with each other, the p–n junction (b-Bi O /Bi O CO )
2 3
O is a p-type semiconductor, while
+
ꢀ
h + H
2
O - OH + H
2
O
2
3
2
3
2
2
3
ꢀ
3À
+
OH + NO - NO + H
2
would be formed when their Fermi levels (EF) reached the
equilibrium state again, and the newly formed energy band
structures would be observed in the interactive structures.
From the above energy band calculations, the possible photo-
catalytic oxidation mechanism of NO on BOC-380 was pre-
sented (Fig. 7). In theory, the photogenerated e on the CB of A b-Bi
4
. Conclusions
À
2
O
3
/Bi
2
O
2
CO
3
composite with a Z-scheme heterojunction
CO
ated h on the VB of Bi O CO migrated to the VB of b-Bi O , precursor at 380 1C. The photocatalytic activities were evaluated
Bi
2
O
2
CO
3
migrated to the CB of b-Bi
2
O
3
and the photogener- was successfully fabricated by the heat treatment of a Bi
2
O
2
3
+
2
2
3
2 3
which led to more accumulated electrons hardly migrating and compared with the photocatalytic oxidation of NO under
ꢀ
À
from O
observed to be beneficial to produce more O
the results of ESR. Therefore, the built-in electric field created temperature-Bi
2
to
O
2
(À0.33 eV). However, the BOC-380 was visible-light irradiation. The b-Bi O /Bi O CO composite exhibited
2
3
2
2
3
ꢀ
À
2
according to much higher photocatalytic activity than pure-Bi
CO . Furthermore, the Z-scheme heterojunction
/Bi CO could facilitate the separation of the
2 2 3
O CO and other
2
O
2
3
during the formation of p–n (b-Bi
2 3 2 2 3
O /Bi O CO ) heterojunctions formation of b-Bi
2
O
3
2
O
2
3
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photogenerated charge carriers, which improved the photocatalytic 17 Y. Liu, Y. Zhou, S. Yu, Z. Xie, Y. Chen, K. Zheng, S. Mossin,
NO removal efficiency eventually.
W. Lin, J. Meng and T. N. Pullerits, ACS Appl. Nano Mater.,
020, 3, 772–781.
2
1
1
8 S. Yao, R. Zheng, R. Li, Y. Chen, X. Zhou, X. Ning, L. Zhan
and J. Luo, J. Am. Ceram. Soc., 2020, 103, 1709–1721.
9 Y. Li, H. Wang, L. Huang, C. Wang, Q. Wang, F. Zhang,
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Conflicts of interest
The authors report no conflicts of interest.
152665–152677.
Acknowledgements
20 D. Zhen, C. Gao, D. Yang, X. Zhu, C. A. Grimes, Y. Liu and
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thanks my family and my friends for their understanding,
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