Dependence of the intrinsic phase structure of Bi2O3catalysts on photocatalytic CO2reduction

Article abstract of DOI:10.1039/d1cy00286d

Rapid recombination of charge carriers and the low efficiency of surface catalysis limit the photocatalytic CO₂reduction performance. Herein, models of Bi₂O₃with different phase structures were investigated to achieve in-depth understanding of the role that phase structure plays in the photocatalytic CO₂process. The gamma phase of Bi₂O₃(γ-Bi₂O₃) exhibited significantly enhanced charge separation ability compared with that of the alpha phase (α-Bi₂O₃) and beta phase (β-Bi₂O₃). Charge-carrier dynamics revealed that the decay lifetime was increased in γ-Bi₂O₃, indicating the enhanced charge carrier separation and migration ability in the γ phase of Bi₂O₃. As expected, the γ-Bi₂O₃photocatalyst exhibited a remarkably improved photocatalytic CO₂reduction activity of 48.10 μmol h^?1g^?1, which was nearly 3.19 and 1.62 times higher than that of α-Bi₂O₃and β-Bi₂O₃, respectively. This work indicates how phase structure affects charge separation and photocatalytic activity, and could open new opportunities for achieving highly efficient photocatalysts and reaction systems.

Full text of DOI:10.1039/d1cy00286d

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Dependence of the intrinsic phase structure of
Bi O catalysts on photocatalytic CO reduction†
2
3
2
Cite this: Catal. Sci. Technol., 2021,
1, 2021
1
Liujin Wei, Guan Huang* and Yajun Zhang *b
ab
a
Received 15th February 2021,
Accepted 1st March 2021
DOI: 10.1039/d1cy00286d
rsc.li/catalysis
4
Rapid recombination of charge carriers and the low efficiency of
difficult and complex. In this regard, structure engineering is
extremely promising for catalytic reaction because it provides
easy and effective regulation of the constitution, charge, and
states of surface atoms.
surface catalysis limit the photocatalytic CO
performance. Herein, models of Bi with different phase
structures were investigated to achieve in-depth understanding
of the role that phase structure plays in the photocatalytic CO
process. The gamma phase of Bi (γ-Bi exhibited
significantly enhanced charge separation ability compared with
that of the alpha phase (α-Bi ) and beta phase (β-Bi ).
Charge-carrier dynamics revealed that the decay lifetime was
increased in γ-Bi , indicating the enhanced charge carrier
separation and migration ability in the γ phase of Bi . As
expected, the γ-Bi photocatalyst exhibited remarkably
improved photocatalytic CO reduction activity of 48.10 μmol h
, which was nearly 3.19 and 1.62 times higher than that of
α-Bi and β-Bi , respectively. This work indicates how phase
2
reduction
2
O
3
2
In general, it is commonly accepted that the crystal-phase
structure of catalysts is a crucial parameter for determination
of their properties. Recently, great efforts have been devoted
to explore the intrinsic mechanisms for the crystal-phase
structure and photocatalytic activity.
relevant reports have been focused on transition element
2
O
3
2 3
O )
2
O
3
2 3
O
5
–9
In addition, most
2
O
3
10–14
2
O
3
metals or metal oxides with different crystal structures.
1
0
2
O
3
a
For example, Ye et al. demonstrated that the photocatalytic
activities of H evolution and CO reduction over cubic
NaNbO were much higher than those of the orthorhombic
structure of NaNbO , which could be attributed to different
−1
2
2
2
−1
g
3
O
2 3
2 3
O
3
11
structure affects charge separation and photocatalytic activity,
and could open new opportunities for achieving highly efficient
photocatalysts and reaction systems.
crystal-phase structures and bandgaps. Zhang et al. reported
that formation of metallic Co nanoparticles improved the C–C
coupling ability of layered double hydroxide-derived catalysts,
which enhanced the selectivity to higher hydrocarbons.
However, the role of main-group metals or metal oxides on
photocharge migration dynamic behavior in phase-structured
Introduction
photocatalysts for CO
As an important main-group metal oxide catalyst, bismuth
oxide (Bi O ) is regarded as the “model” semiconductor, which
2
reduction is rarely reported.
Solar-driven CO
2
conversion is a promising pathway to
simultaneously solve energy issues and environmental
1
,2
problems. Unfortunately, the activity of photocatalytic CO2
reduction suffers from poor efficiency, far below the
requirements of practical applications. The photocatalytic
CO2 reduction reaction takes place on the surface of
semiconductors. The activity is related to light absorption,
2 3
commonly exists in three main crystalline structures:
1
5
α-(monoclinic), β-(tetragonal) or γ-(body-centered cubic).
Among them, the body-centered cubic γ-Bi O phase is, in
2
3
general,
considered to possess relatively excellent
3
photocatalytic performance due to its unique valence band
charge separation and migration, and surface efficiency. In
addition, the high CO dissociation energy of ∼750 kJ mol ,
2
photoreduction of the extremely inert CO molecule is very
−1
structure. α-Bi O is a thermodynamically stable phase and
2 3
2 3 2 3
possesses a smaller bandgap than γ-Bi O , whereas β-Bi O is a
metastable phase and usually transforms into the α-Bi
2 3
O
6
a
School of Chemistry and Chemical Engineering, Guangxi University, Nanning
30004, Guangxi, China. E-mail: huangg66@126.com
phase when the temperature changes. Recently, several
investigations have proved that γ-Bi has disordered
truncated octahedral BiO units and tetrahedral BiO units,
thereby providing more active points.
significant roles of phase structures for Bi
5
b
2 3
O
State Key Laboratory for Oxo Synthesis & Selective Oxidation, Lanzhou Institute
5
5
of Chemical Physics, CAS, Lanzhou, 730000, PR China.
E-mail: yajunzhang@licp.cas.cn
15,16
Despite the
O
2 3
in photocatalysis
†
Electronic supplementary information (ESI) available. See DOI: 10.1039/
d1cy00286d
by controlling the morphology have been reported. However,
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the intrinsic activity of a specific crystal phase in photocatalysis
hampers understanding how a specific phase structure plays a
role in photocharge separation and migration.
structures attributed to α-Bi O (JCPDS card number, 65-2366),
2
3
β-Bi O (JCPDS card number, 78-1793) and γ-Bi O (JCPDS card
2
3
2 3
6,17
number, 74-1375), respectively.
In addition, no characteristic
We wished to clarify the intrinsic activity of the specific
phase structure for Bi O . Hence, highly pure Bi O catalysts
peaks of any other phase and impurities were observed, which
indicated that high-purity and different crystal phase structures
2
3
2 3
with distinctly dominant crystal phase structures (α-Bi
2
O
3
,
2 3
of Bi O samples had been obtained. The corresponding unit
β-Bi O and γ-Bi O ) were fabricated for photocatalytic CO
cell structures are described in Fig. 1d and S3a and b,†
respectively.
2
3
2
3
2
reduction. The photocatalytic activities and time-resolved
reaction intermediate detections were demonstrated to be
owing not only to the specific crystal phase structure, but also
dominated by the surface activity sites, which led to
significant enhancement of catalytic activity. Further transient
photoluminescence and (photo)electrochemical performance
revealed that the γ phase of Bi O enabled charge separation
To further ascertain the chemical compositions and
valence states of as-prepared samples, X-ray photoelectron
spectroscopy (XPS) was undertaken. The peaks corresponding
to the characteristic peaks of Bi and O are clearly shown in
1
8,19
Fig. S4.†
In the Bi 4f region (Fig. S5a†), the peaks around
159.0 and 164.3 eV could be assigned to Bi 4f and Bi 4f5/2
,
2
3
7/2
2
0,21
and migration. As a result, the high selectivity for CO
2
to
respectively.
No obvious peaks of bivalent, tetravalent, or
reduce to CO over γ-Bi O was obtained. Therefore, this work
pentavalent states were found on the Bi 4f7/2 shoulder,
indicating that only trivalent bismuth (Bi III) was present in
the as-prepared samples. The O 1s regions (Fig. S5b†) fitted
into two bands, which at the lower binding energy at ∼530.1
eV corresponded to the lattice O (Bi–O bond), and at a higher
binding energy of ∼532.3 eV could be assigned to surface-
2
3
clearly clarified the controversies on the intrinsic activities for
different crystal phases of Bi catalysts.
2 3
O
Results and discussion
2
2,23
Typical field emission-scanning electron microscopy (FE-SEM)
absorbed oxygen (H O and hydroxyl-like group).
Raman
spectra (Fig. S6†) clearly revealed no obvious change in the
characteristic peaks of as-prepared Bi samples, which
indicated that the different crystal phase structures of Bi O
2
clearly revealed that the preparation of α-Bi O and β-Bi O
2 3
2
3
involved irregular nanoplates (Fig. S1a and b†), and that
γ-Bi O had a hexahedron structure (Fig. 1a). High resolution-
2 3
O
2
3
2 3
transmission electron microscopy (HR-TEM) images (Fig. 1b
and S1c and d†) further exhibited good crystalline and clear
lattice fringes. Specifically, continuous lattice fringes with an
interplanar lattice spacing of 0.325, 0.274 and 0.319 nm could
powders were stable at room temperature after
a
6
,24
hydrothermal process.
the XRD patterns.
These results were consistent with
The actual photocatalytic performance was also evaluated
by photocatalytic CO reduction (Fig. 2a). Notably, the γ-Bi
sample exhibited the highest photocatalytic activity and the
be indexed to the (120) facet of α-Bi
2
O
3
, (220) facet of β-Bi
2
O
3
2
2 3
O
6
and (013) facet of γ-Bi O , respectively. The corresponding
2
3
−
1
−1
phase structures of as-prepared Bi O samples were determined
CO generation rate could reach up to 48.10 μmol h g ,
2
3
by X-ray diffraction (XRD). As shown in Fig. 1c and S2 ,† the
which was nearly 3.19 and 1.62 times higher than that of
preparation of Bi O samples exhibited several crystal phase
α-Bi O
and β-Bi O , respectively. This significant
2 3
2
3
2
3
enhancement activity could be attributed to the highly
exposed active surface in γ-Bi . A trace amount of CH was
generated over as-prepared samples, indicating that evolution
of CH was more difficult than CO formation on the catalyst
surface without a noble metal co-catalyst.
2
O
3
4
4
2
5,26
Based on the
results stated above, we could infer that the preferential two-
electron process for CO evolution was simpler than the eight-
electron reduction of CO
photocatalysts. To further check the carbon source of the
product, an isotope-labelling experiment was done using
2 4 2 3
to CH over pristine Bi O
2
7
1
3
CO
produced a product of CO (m/z = 29), indicating that the
carbon of CO originated from photocatalytic CO reduction
2 2 3
as the substrate gas. As shown in Fig. 2b, γ-Bi O
1
3
2
2
8
over γ-Bi
We wished to reveal the optical properties and charge-
migration ability in the preparation of Bi samples. UV/vis
2 3
O .
2 3
O
absorption spectra (Fig. S7†) revealed the strong absorption
of γ-Bi O in the visible-light range (450–750 nm) in
2
3
comparation with that in other phases. This was due to a
remarkable light-scattering effect in large-scale nanoparticles,
which can generate more activated electrons for
Fig. 1 SEM (a, inset image: bar: 1 μm), HR-TEM (b, inset image: bar: 2
nm), XRD pattern (c) and the corresponding unit cell structure (d) of
1
9,29
γ-Bi
2
O
3
, respectively.
photocatalytic CO
2
processes.
Furthermore, the effects of
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4
γ-Bi O .
To further clarify interfacial charge transfer,
2
3
electrochemical impedance spectroscopy (EIS) measurements
were made for all samples. According to the Nyquist plots
(
Fig. 2f), γ-Bi O exhibited remarkably decreased resistances
2 3
in charge transport compared with those of α-Bi O and
2
3
3
5
β-Bi
2
O
3
.
Thus, these PL and PEC results further verified the
results stated above for CO reduction.
2
To further detect the reaction intermediates during CO2
reduction over as-prepared samples, in situ Fourier-transform
infrared spectroscopy (FT-IR) was done (Fig. 3a–c). Under light
−1
irradiation, the infrared signals in the region 800–2000 cm
increased gradually in intensity in the as-prepared samples due
to the formation of intermediate carbonate species. Specifically,
−1
the absorption bands at 1002 and 1050 cm belonged to the
−1
CH
be attributed to C–OH and HCOOH, respectively.
importantly, the most remarkable difference in the in situ FTIR
spectra for γ-Bi was that the CO* absorption peaks at 1378,
528 and 1628 cm and COOH* absorption band at 1551
3
O* group, whereas the peaks at 1305 and 1723 cm could
36,37
More
2 3
O
2
−1
1
−1
cm , respectively, were part of an intermediate in the
photocatalytic CO reduction for the selective generation of
CO. Moreover, to confirm the CO adsorption capacity in the
2
38
2
as-prepared
samples,
CO
2
temperature-programmed
desorption (CO
desorption temperatures of CO chemisorption on γ-Bi O were
2 2 3
2
-TPD) was carried out (Fig. 3d). All the
2 3
Fig. 2 (a) Average production rates of CO over as-prepared Bi O
13
photocatalysts. (b) Mass spectra of products after CO
γ-Bi , inset image: GC spectra. (c and d) Photoluminescence spectra
and transient photoluminescence (TS-PL) of as-prepared Bi
samples, respectively; (e) chronoamperometric i–t curves in 0.2 mol L
Na SO
2
reduction over
higher than those of α-Bi
result implied that CO
surface more strongly because the surface of γ-Bi O had strong
alkaline active sites due to the specific atom arrangement.
Accordingly, the reaction pathways for photocatalytic CO
reduction over γ-Bi O are briefly described in Scheme 1 and
O
2 3
2 3
and β-Bi O , respectively. This
2
O
3
molecules were binding with the
2
O
3
2
−
1
2
3
2
4
at −0.6 V (vs. SCE) with periodic UV/vis light irradiation (interval
39–41
of 20 s) of different photoanodes; (f) electrochemical impedance
spectroscopy (EIS) of as-prepared samples.
2
2
3
2
in the following steps. First, a CO molecule is absorbed on
the catalyst surface. Meanwhile, a water molecule dissociates
into hydroxyl and hydrogen ions on the surface. Then, the
charge separation and migration capability over different
crystal phases were investigated by steady photoluminescence
(PL) and time-resolved transient photoluminescence (TS-PL).
As shown in Fig. 2c, compared with α-Bi O and β-Bi O , the
2
3
2 3
2 3
PL peak intensity of γ-Bi O was significantly reduced,
indicating that appropriate phase structure could effectively
restrain the charge recombination. Transient PL spectra
2 3
(Fig. 2d) further demonstrated that γ-Bi O possessed a
higher lifetime (τγ-Bi O3 = 53.50 ns) than that of α-Bi
2 3
O (τα-Bi O3
2
2
=
47.10 ns) or β-Bi O (τβ-Bi2O3 = 49.50 ns), respectively,
2 3
3
0,31
indicating the retarded charge combination in γ-Bi
2 3
O .
The photoelectrochemical (PEC) activities of as-prepared
−
1
photocatalysts were evaluated in 0.2 mol
L
Na SO
2 4
−
2
electrolyte under xenon-lamp irradiation (300 mW cm ).
Linear sweeping voltammograms (LSVs, Fig. S8†) and
chronoamperometric i–t curves (Fig. 2e) clearly indicated that
the γ-Bi
density than that of α-Bi
indicating highly efficient (photo)electrochemical activities in
2
O
3
sample exhibited a much higher photocurrent
2
O
3
and β-Bi , respectively,
2 3
O
3
2,33
γ-Bi
γ-Bi
2
O
O
3
3
.
Moreover, as shown in Fig. S9,† the Tafel slope of
−
1
2
was calculated to be 5 mV dec , much lower than
that of α-Bi O (100 mV dec ) and β-Bi O (50 mV dec ),
Fig. 3 In situ FT-IR spectra for a mixture of CO
2 2
and H O vapor over
−
1
−1
2
3
2 3
α-Bi O3 (a), β-Bi O3 (b) and γ-Bi O3 (c) (time interval: 3 min); (d) CO2-
2
2
2
respectively, indicating more efficient catalytic activity over
TPD spectra of as-prepared samples.
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2 3
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