Facet Effects of Ag3PO4 on Charge-Carrier Dynamics: Trade-Off Between Photocatalytic Activity and Charge-Carrier Lifetime

Article abstract of DOI:10.1002/chem.201803505

Silver phosphate (Ag₃PO₄) is a promising visible-light-driven photocatalyst with a strong oxidation power and exceptionally high apparent quantum yield of O₂ evolution. Although engineering Ag₃PO₄ facets is widely known to enhance its photocatalytic activity, most studies have explained its facet effect by calculating surface energies. Herein, the charge carrier dynamics in three kinds of Ag₃PO₄ crystals (mixed facets, cubic, and tetrahedral structures) were first investigated using single-particle photoluminescence microscopy and femtosecond time-resolved diffuse reflectance spectroscopy. As a result, we clarified that the disagreement between the photocatalytic activities (dye degradation and O₂ evolution) of different Ag₃PO₄ facets are the consequence of trade-off between catalytic activity and lifetime of photogenerated charge carriers in addition to surface energy.

Full text of DOI:10.1002/chem.201803505

A Journal of
Accepted Article
Title: Facet Effects of Ag₃PO₄ on Charge Carrier Dynamics: Trade-Off
between Photocatalytic Activity and Charge Carrier Lifetime
Authors: Sooyeon Kim, Yue Wang, Mingshan Zhu, Mamoru Fujitsuka,
and Tetsuro Majima
This manuscript has been accepted after peer review and appears as an
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To be cited as: Chem. Eur. J. 10.1002/chem.201803505
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Facet Effects of Ag3PO4 on Charge Carrier Dynamics: Trade-Off
between Photocatalytic Activity and Charge Carrier Lifetime
Sooyeon Kim,† Yue Wang, Mingshan Zhu, Mamoru Fujitsuka, and Tetsuro Majima*
Abstract: Silver phosphate (Ag3PO4) is a promising visible-light-
driven photocatalyst with a strong oxidation power and exceptionally
high apparent quantum yield of O2 evolution. Although engineering
Ag3PO4 facets is widely known to enhance its photocatalytic activity,
most studies have explained its facet effect by calculating surface
energies. Herein, the charge carrier dynamics in three kinds of
Ag3PO4 crystals (mixed facets, cubic, and tetrahedral structures) were
first investigated using single-particle photoluminescence microscopy
and femtosecond time-resolved diffuse reflectance spectroscopy. As
a result, we clarified that the disagreement between the photocatalytic
activities (dye degradation and O2 evolution) of different Ag3PO4
facets are the consequence of trade-off between catalytic activity and
lifetime of photogenerated charge carriers in addition to surface
energy.
as a photocatalyst. Furthermore, a careful investigation of dye
degradation and O2 evolution of Ag3PO4 is required, as they
cannot be explained by a single factor such as the surface energy
of the facet. To the best of our knowledge, there has been no
report on the direct monitoring of photogenerated charge carriers
of various Ag3PO4 crystals, which may have prevented the further
development of Ag3PO4 as an O2-evolution catalyst.
In this study, sub-micrometer- to micrometer-sized Ag3PO4
crystals with mixed facets (noted Ag3PO4 mixed facets later),
cubic, and tetrahedral structures are thoroughly investigated to
understand their photocatalytic redox activities based on charge
carrier dynamics. We first prepared three kinds of Ag3PO4
samples (mixed facets, cube, and tetrahedron), as described in
the Supporting Information (SI). As shown in Figures 1a-1c,
Ag3PO4 mixed facets have particle-like morphology with smooth
surfaces, whereas Ag3PO4 cube and tetrahedron exhibit sharp
edges and corners. From a Brunauer–Emmett–Teller (BET) test,
the specific surface areas of Ag3PO4 mixed facets and
tetrahedron are found to be nearly the same (1.18 and 1.10 m2
g−1, respectively), whereas that of cube is approximately 3 times
smaller (0.38 m2 g−1). This result well agrees with the obtained
averaged side lengths from SEM images (Table S1). In
accordance with previous reports, all three Ag3PO4 samples have
visible light absorption at over 500 nm (Figure S1a), and the XRD
and XPS results well represent the corresponding Ag3PO4
structures with high crystallinity (Figure S1b and S2, respectively).
Silver phosphate (Ag3PO4) has emerged as a promising O2-
evolving photocatalyst with its bandgap (app. 2.4 eV) and deep
valence band (+2.9 V vs. NHE) with an exceptionally high
apparent quantum yield of O2 evolution (over 80% at λ < 480
nm).[1] Because photocatalytic activity is greatly influenced by
surface energy and area, presence of defect sites, and charge
carrier lifetime, sophisticated and rational material designs are
required to improve its catalytic activity. Among various
approaches, crystal facet engineering has been widely applied to
many photocatalytic semiconductor materials because surface
energy and charge carrier dynamics are greatly influenced by
facet and structure.[2]
There have been great efforts to enhance the Ag3PO4
photocatalytic performance. Bi et al. reported the synthesis of
Ag3PO4 rhombic dodecahedron and cube with sharp corners and
edges.[3] Due to the higher surface energy of the (110) facets, a
rhombic dodecahedron shows higher activities of dye degradation
than a cube. In addition, Martin et al. reported that the Ag3PO4
tetrahedron with (111) facet showed the highest photocatalytic
activities for O2 evolution, followed by mixed facets, cube, and
rhombic dodecahedron.[4] Conversely, Hsieh et al. recently
reported that the Ag3PO4 tetrahedron was nearly inert for dye
degradation, whereas the Ag3PO4 cube generated the largest
amount of hydroxyl radical (•OH).[5] Thus, there has been no
consensus on which crystal structure of Ag3PO4 is advantageous
Dr. S. Kim, Y. Wang, Dr. M. Zhu, Prof. M. Fujitsuka, Prof. T. Majima
The Institute of Scientific and Industrial Research (SANKEN)
Osaka University, Mihogaoka 8-1, Ibaraki, Osaka 567-0047 (Japan)
* Corresponding author. E-mail: majima@sanken.osaka-u.ac.jp
Figure 1. SEM pictures of Ag3PO4 mixed facets (a), cube (b), and tetrahedron
(c) (scale bar: 1 μm). Photocatalytic formation of resorufin (d) and O2 evolution
(e) in aqueous solution using Ag3PO4 mixed facet (black, circle), cube (red,
square), and tetrahedron (blue, triangle). All tests were conducted under
visible light irradiation (λ > 420 nm, 480 mW cm−2). Five-percent methanol was
added in the oxidation test of amplex red to decelerate resorufin formation and
dye degradation (b). To improve photostability of Ag3PO4 without an electron
† Present address: Laboratory for Cell System Control, Center for
Biosystem Dynamics Research, RIKEN, 6-2-3 Furuedai, Suita,
Osaka, 565-0874, Japan
Supporting information for this article is given via a link at the end of
the document.
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scavenger (50 mM AgNO3), we employed the phosphate buffer condition
containing sufficient [PO4]−.[6]
tetrahedron, leading to faster charge recombination than that of
cube.[5]
Amplex red was employed to evaluate the photocatalytic •OH
formation by three Ag3PO4 samples (Figure S3).[7] Pink-colored
resorufin was formed by the oxidation of amplex red chromophore
by •OH (Figure S3), which can be detected by the appearance of
absorbance at around 572 nm (Figure S4a). Under visible light
irradiation (λ > 420 nm), it was revealed that the Ag3PO4
tetrahedron induced amplex red oxidation the fastest, whereas
the Ag3PO4 mixed facet and cube oxidized amplex red 5 times
slowly (Figure 1d). Furthermore, O2 evolution tests were
performed for three Ag3PO4 samples under visible light irradiation.
Contrary to the amplex red assay, the rates of photocatalytic O2
generation of Ag3PO4 mixed facets, cube, and tetrahedron did not
differ significantly regardless of the presence of an electron
scavenger (50 mM silver nitrate, Figure 1e). During our repetitive
experiments, the overall trends were not altered by elongated
irradiation (Figure S5).
As previously reported, Ag3PO4 tetrahedron has been
considered as a highly active photocatalytic crystal due to its
higher surface energy than that of Ag3PO4 cube and rhombic
dodecahedron.[4] Nonetheless, our results indicate that surface
energy cannot solely explain the disagreement between the
photocatalytic activities of Ag3PO4 samples. Previously, we did
reveal that the (001) facet of TiO2 is a more active site for
photocatalytic reduction than the (101) facet although the (101)
facet exhibits higher surface energy.[2a] Furthermore, the
enhancement in photocatalytic activity by sharp corners and
edges[8] was not observed in our study, as the Ag3PO4 mixed
facets showed similar activities as those of the Ag3PO4 cube and
tetrahedron (Figure 1e). Therefore, several factors that may affect
the photocatalytic activities of Ag3PO4 should be considered
together on the basis of time-resolved spectroscopic
measurements.
Figure 2. TDR spectra of Ag3PO4 mixed facets (a), cube (b), and tetrahedron
(c) taken after 5, 20, 46, 106, 206, 506, and 1046 ps of a femtosecond-pulse
excitation (λex = 400 nm). (d) Normalized TDR decays of Ag3PO4 mixed facets
(black), cube (red), and tetrahedron (blue) monitored at around 950 nm. Green
lines show results of double-exponential fitting. The fitting parameters are
summarized in Table 1.
Table 1. TDR fitting parameters[a]
A1 / %
33 ± 1
16 ± 2
39 ± 1
τ1 / ps
A2 / %
37 ± 1
35 ± 2
33 ± 1
τ2 / ps
A3 / %
28 ± 1
47 ± 3
23 ± 1
Mixed facets
Cube
37.7
2.5
±
±
±
584.6
55.4
837.3
9.2
±
±
±
50.8
9.2
Tetrahedron
19.1
1.1
434.9
31.2
In Figure 2, the transient absorption spectra of three
Ag3PO4 samples upon 400-nm excitation were measured in the
near-infrared (NIR) region using femtosecond time-resolved
diffuse reflectance (TDR) spectroscopy. Considering the broad
spectral shapes and energy of the transient species,[9] we
assigned the observed transient species to the photogenerated
electrons in Ag3PO4. The decay of the charge carriers was well
fitted with a double-exponential function, as summarized in Table
1. Ag3PO4 mixed facets, cube, and tetrahedron underwent a rapid
relaxation (τ1 = 37.7, 50.8, and 19.1 ps, respectively) followed by
slower decays in the sub-ns time scale (τ2 = 584.6, 837.3, and
434.9 ps, respectively). The observed relaxation processes
cannot be explained by bimolecular charge recombination
between hole and electron, which usually follow power law
kinetics. Because photocatalytic reactions such as water
oxidation are reported to occur in the millisecond time scale,[10]
the observed kinetics represent complicated relaxation processes
such as charge trapping and recombination before diffusion-
limited reactions occur. When the three decay profiles were
compared together (Figure 2d), the Ag3PO4 tetrahedron exhibited
the fastest relaxation pathway of the photogenerated electron
(19.1 ps, 39%). The proportion of the remaining electrons at over
1 ns was the largest for cube, followed by mixed facet and
tetrahedron (58.5, 34.8, and 27.5%, respectively). This result
agrees with the results of Hsieh et al. that the highest barrier for
electron transport exists on the (111) crystal facet of the Ag3PO4
[a] Three decay profiles (Figure 2d) were well fitted by a double exponential
function; y = A1exp(-x/τ1) + A2exp(-x/τ2) + A3.
To investigate the underlying mechanisms of the facet and
the structural effects on photocatalytic activities, single-particle
photoluminescence (PL) microscopy was used to monitor the PL
properties of Ag3PO4. This method can clearly visualize the local
active site on the single particle and hidden photocatalytic
mechanisms, which are not accessible through ensemble-
averaged photocatalytic experiments.[11] Figures 3a-3c show the
representative PL lifetime images of Ag3PO4 mixed facets,
tetrahedron, and cube, and additional results can be found in
Figures S6 and S7. Interestingly, there were common
characteristics between the lifetime and energy of Ag3PO4 single-
particle PL; as the PL energy increases (i.e., blue-shifted emission
spectra), the PL lifetime becomes shorter. As shown in Figure 4,
the maximums of the PL spectra with short (τ < 0.2 ns) and long
lifetime (2.5 ns < τ < 5.0 ns) were approximately 460 and 750 nm,
respectively. Considering the band-gap energy of Ag3PO4 (app.
2.6 eV, Table S1), the former represents band edge emission, and
the latter represents NIR emission, which is presumably induced
by the relaxation of charge trapping states. Such heterogeneity in
PL lifetime/energies was most apparent in Ag3PO4 mixed facets
(Figures 3 and S6). On careful comparison of single-particle PL
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Figure 3. Representative single particle PL lifetime images of (a) Ag3PO4 mixed facet, (b) cube, and (c) tetrahedron (λex = 405 nm) taken in air and (insets)
corresponding SEM pictures (scale bar: 1 μm). (e-f) Single particle PL spectra measured at the points indicated by arrows in (a) and (b) or at the center of a
single Ag3PO4 tetrahedron (c). Incomplete spatial matching between SEM and PL images is due to photocorrosion or slight displacement of Ag3PO4 samples
under the vacuum condition of SEM measurement.
lifetime and SEM images, the sites with short PL lifetime were
where the phosphorus-oxygen bond is omitted in eq 2. In light
found to be located on the defect-like surfaces or grain boundaries. of the previous study, the Ag atoms on the (100) surface are
This spatial correlation implies that the photogenerated electron
in the Ag3PO4 mixed facets in the structural defect undergoes
rapid charge recombination. Besides, the charges on the smooth
surfaces of Ag3PO4 mixed facets are slowly relaxed, resulting in
charge recombination in the nanosecond time scale.
coordinatively saturated, whereas the Ag atoms on the (111)
surface are located at three-coordinated sites with one dangling
bond.[12] Thus, the STH residing on the (111) surface
([Ag2=O•••Ag]surf+ in eq 2) would be less stable than those on the
fully coordinated (100) surface. Consequently, the hole on the
(111) facet has
photogenerated electron or oxidize nearby substances than that
on the (100) facet.
a greater tendency to recombine with
On the other hand, we initially supposed that the sharp
corners of the Ag3PO4 cube and tetrahedron would be strongly
emissive because the corners and edges of the semiconductor
have intrinsically more defect sites and act as reactive sites and
charge recombination centers of the photocatalyst. As shown in
Figures 3b and 3c, however, strong PL of the Ag3PO4 cube PL
was detected at certain sites on the planes and edges, whereas
the entire plane of the Ag3PO4 tetrahedron was emissive without
a particular spatial dependency. Another noteworthy finding is
that the PL intensities and spectra of the Ag3PO4 cube were
largely heterogeneous by particles, which was not evident in the
Ag3PO4 tetrahedron; the PL intensity, lifetime, and spectrum of
Indeed, the decay of photogenerated electron was the
fastest in the Ag3PO4 tetrahedron, and no spatially preferential
charge recombination was observed. This phenomenon can be
explained by the short-lived and reactive STH on the (111) facets.
Once the photogenerated charge carriers are trapped on the
(111) facets, most of them probably undergo charge
recombination, which conversely prevents photocorrosion (Figure
S8).[13] From single-particle PL measurements, these shallow
traps are found to have comparable energies of the Ag3PO4
the Ag3PO4 tetrahedron did not deviate based on sites or particles. bandgap. It should be emphasized that we did not observe any
NIR emission from the Ag3PO4 tetrahedron; hence, the deep trap
To elucidate the observed properties of Ag3PO4, we
is not dominant on the (111) facets. When considered together,
propose that there are two types of surface trapped holes (STH)
the charge recombination kinetics of a few tens and hundreds of
in Ag3PO4 depending on its facets: a hole either in a short-lived
picoseconds obtained in the TDR measurements represent the
and reactive ‘shallow trap’ or in a relatively more stable and less
process of charge carrier migration to the surface and trapping in
reactive ‘deep trap’ (Figure 4). It has been reported that the
the ‘shallow traps’ (kCR1 and kCR2 in Figure 4b, respectively). In
conduction and valence bands (CB and VB, respectively) of
addition to the charge carrier dynamics described above, the
Ag3PO4 are composed of Ag 5s5p with a small quantity of P 3s
(111) facets exhibit over-abundance of dangling phosphorus-
orbitals and Ag 4d with O 2p orbitals, respectively.[1] Thus, upon
oxygen bonds, which act as oxidation sites, thus further
photoirradiation, we expect charge separation (eq 1) and
contributing to the strong photocatalytic oxidation ability of the
subsequent formation of STH (eq 2) in Ag3PO4, as given below.
Ag3PO4 tetrahedron.[14]
Ag3PO4 + hν → Ag3PO4 + h+ + e-
(1)
Meanwhile, the ‘deep traps’ are considered to be mostly
located on the fully saturated Ag. As shown in single-particle PL
[Ag2=O‒Ag]surf + h+ → [Ag2=O•••Ag]surf
,
(2)
+
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resulting in significant photocorrosion. Such surface roughening
has been reported in rutile TiO2, induced by nucleophilic attack of
an H2O molecule on the STH.[16] Interestingly, we did observe
fluctuation of single-particle PL intensity of Ag3PO4 mixed facets
and shortening of single-particle PL lifetime, indicating in situ
formation of defect sites and shallow traps on the smooth surface
due to the cleavage of the coordination bonds of Ag (Figure S10).
In conclusion, we have thoroughly investigated
photocatalytic activities, kinetics of photogenerated charge
carriers, and single-particle PL behaviors of Ag3PO4 depending
on its facets. Here, we first demonstrated the presence and
distribution of different trap sites on the (100) and (111) facets of
Ag3PO4. The different photocatalytic activities of the (111) and
•
(100) facets to generate OH and O2 (Figures 1d and 1e) can
presumably be attributed to the proportion of shallow traps with a
higher oxidation ability since •OH formation requires higher
oxidation potential than O2 evolution (2.83 and 1.23 eV vs NHE,
respectively).[17] Nonetheless, STH on the (111) facets are less
stable, resulting in facile charge recombination. These results
indicate a trade-off relationship between charge carrier lifetime
and photocatalytic activity; long-lived charge carriers are
sometimes too stable to react. The obtained insights will
contribute toward improving the photostability of Ag3PO4, which is
a major drawback of Ag3PO4 in practical applications, and
designing more sophisticated photocatalysts to trigger a selective
oxidation process for biological and medical applications (e.g.,
Figure 4. Charge carrier kinetics and different types of traps depending on the
Ag3PO4 facets revealed in this study. ST and DT denote shallow and deep traps,
respectively. kCR indicates the rate constant of charge recombination obtained
from the TDR measurements, whereas kDT,r and kST,r are the rate constants of
the radiative recombination processes of the deep and shallow traps,
respectively, calculated from single-particle PL measurements.
•
selective O2 evolution during water oxidation with negligible OH
formation).
Acknowledgements
We thank Prof. T. Sekino, Dr. S. Cho, Mr. Y. Seo, Dr. O. Elbanna,
Ms. C. Cai (ISIR, Osaka University), Prof. H. Yamashita, and Dr.
Y. Kuwahara (Graduate School of Engineering, Osaka University)
for their advice and assistance in the synthesis and
characterization of Ag3PO4. This work was partly supported by a
Grant-in-Aid for Scientific Research (Project 25220806 and
others) from the Ministry of Education, Culture, Sports, Science,
and Technology (MEXT) of the Japanese Government.
images, long-lived deep traps were populated on the smooth
surfaces of Ag3PO4 mixed facets and cube samples. From their
spatially distinguished NIR emissions, the energy of the
photogenerated charge carriers in the deep traps would be
approximately 0.6–1.0 eV smaller than in the Ag3PO4 bandgap.
Because the Ag3PO4 mixed facets and cube enable the same
photocatalytic oxidation reaction as that of the tetrahedron, we
expect that the energy level of the deep trap should be sufficient
for water oxidation. Thus, 0.6–1.0 eV smaller energy originates
from both trap sites of electron and hole, as depicted in Figure 4a.
Based on the results of the TDR measurements, a few hundreds
of picosecond kinetics represents the trapping of charge carriers
in less reactive deep traps (kCR2 in Figure 4a). On the other hand,
short-lifetime and band-edge PL was observed in the defect sites
and grain boundaries of Ag3PO4 mixed facets and cubes,
indicating that the STH in the imperfect crystalline region
(analogous to shallow traps of (111) facets) undergo rapid charge
recombination (kST,R in Figure 4a). While the role of grain
boundaries in the charge carrier lifetime are varied depending on
the photocatalyst materials,[15] the grain boundaries of Ag3PO4
mixed facets accelerated the charge recombination process.
We further claim that the long-lived photogenerated charge
Keywords: Photocatalysis • Silver phosphate • Water splitting •
Charge carrier dynamics • Single particle photoluminescence
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Entry for the Table of Contents (Please choose one layout)
Layout 1:
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Revisit Ag3PO4 facet effects Distinct
charge carrier kinetics on (111) and
(100) facets of Ag3PO4 were clearly
elucidated at picosecond and single-
particle resolution.
Sooyeon Kim, Yue Wang, Mingshan
Zhu, Mamoru Fujitsuka, and Tetsuro
Majima*
Page No. – Page No.
Facet Effects of Ag3PO4 on Charge
Carrier Dynamics: Trade-Off between
Photocatalytic Activity and Charge
Carrier Lifetime
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