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org/JPCL Perspective

In Situ Irradiated X‑ray Photoelectron Spectroscopy Investigation on

Electron Transfer Mechanism in S‑Scheme Photocatalyst
Jianjun Zhang, Liuyang Zhang, Wang Wang,* and Jiaguo Yu*

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ABSTRACT: S-scheme photocatalysts have demonstrated great potential in solar fuel

production. To study the electron transfer pathways in S-scheme heterojunctions, in situ
irradiated X-ray photoelectron spectroscopy (ISIXPS) is an effective and widely used
technology. However, the mechanism of ISIXPS in identifying the electron transfer pathways
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in S-scheme heterojunction has not yet been elucidated. In this Perspective, the development
process and the formation mechanism of S-scheme photocatalysts are first introduced.
Afterward, the principles of XPS and ISIXPS measurements are thoroughly explained, and
the applications of XPS and ISIXPS in confirming the interfacial electron transfer in S-
scheme heterojunctions are discussed. Finally, suggestions for future research on the
utilization of ISIXPS in S-scheme heterojunctions are proposed. This Perspective will provide
deep insight into the electron transfer mechanism in S-scheme photocatalysts through
ISIXPS.

T he energy demand is growing because of rapid economic

and social development. The overexploitation and
consumption of fossil fuels have caused an energy crisis and
From the viewpoint of dynamics, the repulsion between the
electrons (or holes) in SI and electrons (or holes) in SII and the
electron−hole attraction hinder the charge transfer between SI
environmental pollution.1−4 To achieve carbon neutrality, the and SII. To improve the redox capacity of the photocatalytic
shift from fossil fuels to renewable energy is essential. Solar systems, inspired by the natural photosynthesis of plants, Bard
energy is a clean and abundant renewable energy source.5−7 proposed traditional (liquid) Z-scheme systems with suitable
Emerging semiconductor photocatalysis is one of the most redox ion pairs (RIPs) in 1979.16 The RIPs generally consist of
promising technologies for solar energy utilization. Photo-
an electron acceptor and an electron donor (taking Fe3+/Fe2+ as
catalytic water splitting and photocatalytic CO2 reduction can
an example). After careful consideration, the supposed electron
convert solar energy into storable and transportable chemical
fuels (also known as solar fuels, such as hydrogenand methanol) transfer pathway in traditional Z-scheme systems is found to be
at ambient temperature and pressure.8−10 incorrect (Figure 1b). From the perspective of thermodynamics
Currently, the key scientific problem in photocatalysis is the and electrochemistry, Fe3+ is more likely to accept electrons
rapid recombination of photogenerated electrons and from the CB of SII, whereas Fe2+ is more easily oxidized by the
holes.11−13 For single semiconductor photocatalysts, the holes in SI. Besides, the existence of RIPs confines the
photogenerated carriers are easily recombined inside photo- application of traditional Z-scheme systems to the liquid
catalysts because of the strong Columbic interaction between phase. To remove this restriction, an all-solid-state Z-scheme
electrons and holes. To suppress the recombination of heterojunction was proposed by Tada et al. in 2006.17 Solid
photogenerated carriers in single photocatalysts, coupling two metal conductors are used to replace the RIPs, extending the
semiconductors has been confirmed to be an effective application of Z-scheme photocatalysts to gas/solid-phase
strategy.14,15 For a long time, numerous researchers have used reactions. However, the electron transfer pathway in all-solid-
type-II heterojunctions to explain the electron transfer state Z-scheme heterojunction still has the same problem as that
mechanism in these composite photocatalysts. As exhibited in in the traditional Z-scheme systems.
Figure 1a, under photoexcitation, photogenerated electrons
transfer from the conduction band (CB) of semiconductor II
(SII) to the CB of semiconductor I (SI), while photogenerated Received: July 7, 2022
holes transfer from the valence band (VB) of SI to the VB of SII. Accepted: August 31, 2022
Although type-II heterojunctions seem to spatially separate Published: September 2, 2022
photogenerated carriers, they are faced with some problems.
Thermodynamically, the electron and hole transfer pathways
lead to decreased redox capacity of the photocatalytic systems.

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will transfer from RS to OS until an equilibrium state is reached

(Figure 2b). Accordingly, the energy bands near the RS interface
are bent upward and the RS interface is positively charged
because of the depletion of electrons. In contrast, the energy
bands near the OS interface are bent downward and the OS
interface is negatively charged owing to the acceptance of
electrons. Therefore, a built-in electric field (BEF) is generated
at the interface with the direction pointing from RS to OS.
Additionally, the Ef near the RS interface gradually decreases and
the Ef near the OS interface gradually increases until the same
point is reached. Under photoexcitation, electrons are excited
into the CB and holes are generated in VB. The photogenerated
electrons in the CB of OS will transfer to the VB of RS driven by
the BEF (Figure 2c). Furthermore, the photogenerated electron
in the CB of RS will transfer to the surface of RS because of the
action of BEF. In contrast, the photogenerated holes in the VB of
RS will transfer to the interface of OS to recombine with the
photogenerated electrons of OS driven by the BEF (Figure 2c).
Also, the photogenerated holes in the VB of OS will further
transfer to the surface of OS. Consequently, the electrons with
strong reduction ability in the CB of RS and holes with superb
oxidation ability in the VB of OS are retained and separated in S-
scheme heterojunctions.
To verify the electron transfer pathways in S-scheme
photocatalysts, in situ irradiated X-ray photoelectron spectros-
Figure 1. (a) Charge transfer pathways in type-II heterojunction and its copy (ISIXPS) is a powerful tool.21,22 However, the principle of
problems: Thermodynamically, the redox ability is weakened; ISIXPS has not yet been revealed. This Perspective will provide
dynamically, the interelectron (or interhole) repulsion hinders the
supposed electron (or hole) transfer. (b) Supposed (solid lines) and
detailed explanations of the mechanism of XPS and ISIXPS in
actual (dotted lines) charge transfer pathways in traditional Z-scheme evaluating the electron transfer in S-scheme heterojunctions.
heterojunction. Thermodynamically, the supposed electron transfer Before discussing the applications of ISIXPS, it is important to
pathway is wrong. The actual electron transfer pathway is from CB of understand the fundamentals of XPS. XPS is an advanced and
SII to RIPs to VB of SI. sensitive surface analysis technology, which can provide
information on the elemental composition and content,
To resolve the problems and shortcomings of type-II chemical state, and chemical bonding of various compounds.23
heterojunction and Z-scheme heterojunctions, our group As is known to all, substances are composed of atoms, molecules,
proposed a new concept of S-scheme (step-scheme) hetero- and ions. Molecules and ions are formed through the covalent or
junction in 2019.18,19 An S-scheme heterojunction photocatalyst ionic bonding of atoms. Furthermore, an atom is made up of a
is generally composed of a reduction semiconductor (RS) nucleus and electrons that are constantly moving in atomic
photocatalyst and an oxidation semiconductor (OS) photo- orbitals around the nucleus. During XPS measurements, a solid
catalyst with a staggered band structure.20 Prerequisites for the sample electrically connected to the equipment is placed in a
formation of the S-scheme heterojunction are that both the CB chamber with an ultrahigh vacuum (<10−9 Pa). When the
and Ef positions of RS are higher than those of OS. Herein, we sample surface is irradiated by a beam of high-energy X-rays
analyze the formation process of S-scheme heterojunction for (1486.6 eV for Al Kα X-rays), the excited electrons are able to
two n-type semiconductors. Since RS possesses higher Ef than escape from the sample surface into the vacuum (also known as
OS (Figure 2a), when RS and OS are in close contact, electrons the photoelectric effect), causing ionization of the atoms (Figure

Figure 2. Formation process of S-scheme heterojunction photocatalyst: (a) positions of the energy bands and Ef before contact; (b) generation of BEF
and band bending near the interface after contact; (c) transfer pathway of photogenerated carriers under photoexcitation. The photogenerated
electrons will transfer from the CB of OS to the VB of RS driven by the BEF.

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Figure 3. (a) Principle of XPS measurements. When X-rays irradiate the sample surface, the excited electrons will escape from the sample surface and
enter the analyzer. (b) Generation process of photoelectron during XPS measurements. The excited electrons have sufficient energy to break through
the restrictions of Eb and Ws and escape from the sample surface with Eb. (c−e) Structures of carbon atoms after losing or accepting an electron. The Eb
of C 1s is increased when losing one electron, and the Eb of C 1s is decreased when accepting one electron.

Figure 4. (a) Principle of ISIXPS measurements. X-rays and UV−vis light simultaneously irradiate the sample surface, and photoelectrons are collected
by an analyzer. (b) Excitation processes of electrons during ISIXPS measurements. X-rays can excite the inner-shell electrons to become free
photoelectrons with Ek, while UV−vis light can only excite the valence electrons in the energy levels of VB into the energy levels of CB. (c) Changes in
electron density and elemental Eb of S-scheme photocatalyst under photoexcitation. Decreased electron density of OS leads to the increased elemental
Eb, while increased electron density of OS causes the reduced elemental Eb.

3a). The emitted electrons (photoelectrons) with different (from close to far), the independent atomic orbitals around the
kinetic energy (Ek) will pass the analysis slit of the XPS device, nucleus can be divided into different orbitals such as 1s, 2s, 2p,
and the electron current (related to the number of photo- and 3s. The energy required to eject an electron from the sample
electrons per unit time), which depends on Ek, can be is known as the electron’s ionization energy or binding energy
recorded.24 A vivid description of the above-mentioned process (Eb). Specifially, electrons in inner orbitals (such as 1s orbital)
is illustrated in Figure 3b. From a microscopic perspective, the have a higher Eb than those in outer orbitals (such as 2p orbital).
energy of atomic orbitals is quantized, and thus, each electron X-rays can excite the inner-shell electrons because of their
has a discrete energy. According to the distance from the nucleus extremely high energy (for instance, Al Kα X-rays have an hν of
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Figure 5. High-resolution XPS spectra of (a) C 1s in PT, CP, and CP under UV irradiation. High-resolution XPS spectra of (b) Cd 3d and (c) S 2p in
CdS, CP, and CP under UV irradiation. (d) Formation process of CdS/PT S-scheme heterojunction. Reproduced with permission from ref 27.
Copyright 2021, Wiley-VCH.

1486.6 eV). The excited electrons thus possess sufficient energy occurs in covalent compounds and new molecular orbitals are
to break through the restrictions of the Eb and the work function formed, leading to a redistribution of electrons and a change in
of sample (Ws), and finally escape from the sample surface with electron density. Therefore, the Eb of C 1s will also change when
Ek. Therefore, the Eb can be calculated by the following format:25 the carbon atom is in different chemical environments. The Eb of
C 1s increases when the electron density decreases in a carbon
E b = hv Ek Ws atom, while the Eb of C 1s decreases when the electron density
In practical XPS measurements, the Eb of inner-shell electrons increases in a carbon atom. Although this kind of change in Eb is
can be obtained through measuring the Ek of photoelectrons. relatively smaller than that of electron acceptance or loss, the
Subsequently, the elements contained in the sample can be consequent chemical shift is detectable in XPS.
identified based on the value of Eb, because the Eb is almost With the fundamentals of general XPS having been
unique for each element. introduced, the mechanism of ISIXPS measurements is analyzed
Furthermore, the Eb of inner-shell electrons is related to the next. During ISIXPS measurements, the high-energy X-rays and
chemical state of the atom. When electron loss and acceptance ultraviolet−visible (UV−vis) light simultaneously irradiate the
occur in the outer orbitals of an atom, the Eb of inner-shell sample surface (Figure 4a). Subsequently, the excited photo-
electrons is changed (also called chemical shift). Taking the electrons with Ek will escape from the sample surface to the
carbon atom as an example, it possesses two electrons in each of vacuum and be collected by the analyzer. To analyze in detail the
the 1s orbital, 2s orbital, and 2p orbital (Figure 3d). Besides, the functions of UV−vis light on the sample during ISIXPS
carbon nucleus consists of six protons and six neutrons, and thus, measurements, the excitation process of electrons is illustrated
it has six positive charges. The attractive forces between atomic in Figure 4b. X-rays with extremely high energy (Al Kα = 1486.6
nuclei and electrons are Coulombic force and nuclear force. The eV) can excite the inner-shell electrons to overcome the
Coulombic force stems from protons, while the nuclear force is restrictions of Eb and Ws and finally become free photoelectrons
generated by both protons and neutrons. Since the number of with the energy of Ek. However, the energy of UV−vis light (2−4
protons and neutrons in a carbon nucleus is fixed, the attractive eV) is quite low in comparison with the X-ray and can only excite
force that the nucleus can provide is constant. When a carbon the valence electrons from VB to CB, while the excited valence
atom loses one valence electron in the 2p orbital, the total electrons remain bound to the nucleus (Figure 4b). Hence, in
number of electrons bound around the nucleus is reduced to five ISIXPS measurements, the analyzer detects the Eb of inner-shell
(Figure 3c). Considering the atom as a whole, the attractive electrons after the excitation of the outer-shell valence electrons.
force assigned to each electron by the nucleus is enhanced, and The excitation process of valence electrons also corresponds to
thus, the Eb of C 1s increases. In contrast, when a carbon atom the electron transition from VB to CB in semiconductors. The
accepts one electron in its 2p orbital, the total number of excited electrons in the CB are also known as photogenerated
electrons increases to seven. Hence, the attractive force assigned electrons, which remain inside the semiconductors and can
to each electron is weakened and the Eb of C 1s decreases transfer between two semiconductors. Similar to the analysis in
(Figure 3e). In some cases, the acceptance or loss of electrons is normal XPS, the loss of photogenerated electrons will result in
difficult to happen. For example, hybridization of atomic orbitals decreased electron density and increased elemental Eb, whereas
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Figure 6. High-resolution XPS spectra of (a) Ti 2p and (b) O 1s in TiO2, TiO2@ZnIn2S4, and TiO2@ZnIn2S4 under light illumination. High-
resolution XPS spectra of (c) Zn 2p, (d) In 3d, and (e) S 2p in ZnIn2S4, TiO2@ZnIn2S4, and TiO2@ZnIn2S4 under light illumination. (f) Electron
transfer in TiO2@ZnIn2S4 S-scheme heterojunction under light irradiation. Reproduced with permission from ref 21. Copyright 2021, Wiley-VCH.

the acceptance of photogenerated electrons will lead to electron density in RS and reduced electron density in OS
increased electron density and decreased elemental Eb. (Figure 4c). Hence, the elemental Eb of RS decreases, and that of
According to the above discussion, the evidence of electron OS increases within the S-scheme photocatalyst under
transfer in S-scheme heterojunctions under darkness and illumination.
irradiation can be obtained through the combined analysis of Based on the mechanism analysis of XPS and ISIXPS, two
normal XPS and ISIXPS results. The change in Eb of a specific examples are given, employing ISIXPS to disclose the charge
element can be used to estimate the change of electron density. transfer mechanism in S-scheme heterojunctions. Cheng et al.
Therefore, the electron transfer direction in S-scheme reported an inorganic/organic S-scheme heterojunction photo-
heterojunctions can be determined.26 Normal XPS can detect catalyst with high hydrogen production efficiency.27 CdS
the electron transfer between RS and OS when they come into nanocrystals are grown on the surface of pyrene-alt-triphenyl-
contact. Since RS has a higher Ef than OS, electrons will transfer amine conjugated polymer (PT) via a solvothermal process.
from RS to OS after contact. Compared with RS before contact, Both CdS and PT are n-type semiconductors with a staggered
the electron density of RS decreases after contact, and the Eb of band structure, and the CB and Ef positions of PT are higher
constituent elements in RS increase correspondingly. Con- than those of CdS, satisfying the conditions for the formation of
versely, compared with OS before contact, the electron density an S-scheme heterojunction. Normal XPS and ISIXPS measure-
of OS within the S-scheme photocatalyst increases, and the ments are performed to confirm the electron transfer in CdS/PT
elemental Eb of OS should be decreased. Furthermore, ISIXPS (CP) S-scheme photocatalyst. As shown in the high-resolution
can also confirm the transfer direction of photogenerated XPS spectra of C 1s, the peak located at 284.8 eV is the aromatic
electrons in the S-scheme heterojunction. Under photo- sp2 carbon which is used for calibration, and the peak of the C−
excitation, the photogenerated electrons in the CB of OS will N bond in PT is situated at 286.3 eV (Figure 5a). In comparison
transfer to the VB of RS driven by the BEF, leading to increased to PT, the peak of C−N in CP shifts toward higher Eb,
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suggesting that PT loses electrons and its electron density Within S-scheme heterojunctions, the electron density of OS
decreases. In contrast, compared with CdS, both Cd 3d and S 2p should be further reduced and that of RS should be further
peaks of CP shift toward lower Eb (Figure 5b,c), indicating that increased, resulting in a greater shift of the XPS peaks.
CdS obtains electrons from PT and its electron density Therefore, studying the effects of UV−vis light intensity in
increases. The changes in the electron density of CP and CdS ISIXPS measurements can provide additional evidence for
verify the electron transfer from PT to CdS after contact in electron transfer in S-scheme heterojunctions.
darkness (Figure 5d). In ISIXPS measurements, UV light, whose (2) Elucidate the influence of BEF strength on the electron
wavelength is 365 nm, irradiates the sample surface. The peak of transfer in S-scheme heterojunctions. According to the
C−N in CP shifts toward lower Eb, while the peaks of Cd 3d and formation mechanism of the S-scheme heterojunction, the
S 2p in CP move toward higher Eb. This phenomenon indicates BEF strength is related to the difference of Ef between RS and
the electron density increment and decrement in PT and CdS, OS. When the difference of Ef between RS and OS increases, the
respectively, further confirming the electron transfer from CdS BEF strength should be enhanced, leading to a stronger driving
to PT under UV light irradiation. Therefore, normal XPS and force for the interfacial electron transfer. Photogenerated
ISIXPS results successfully reveal the electron transfer pathways electrons are easier to transfer from the CB of OS to the VB
in the CdS/PT S-scheme heterojunction. of RS, bringing about greater changes in the electron density and
In addition, Wang et al. constructed an S-scheme TiO2@ elemental Eb of OS and RS. Hence, further evidence on S-
ZnIn2S4 core−shell photocatalyst with superb photocatalytic scheme heterojunctions can be obtained by studying electron
CO2 reduction performance.21 ZnIn2 S4 nanosheets are transfer in S-scheme photocatalysts with different BEF strengths
deposited on the surface of TiO2 hollow spheres by an in situ through ISIXPS measurements.
chemical bath, and the TiO2@ZnIn2S4 composite also meets the
requirements of constructing S-scheme heterojunctions. Com-
pared with single TiO2, both the identified Ti 2p and O 1s peaks
■ AUTHOR INFORMATION
Corresponding Authors
in TiO2@ZnIn2S4 shift toward lower Eb after contact in darkness
(Figure 6a,b). Conversely, all the peaks of Zn 2p, In 3d, and S 2p Wang Wang − Department of Chemistry, Wuhan University,
move toward higher Eb compared with single ZnIn2S4 (Figure Wuhan 430072, P.R. China; Email: doublewang@
6c−e). These results suggest that the electron density of TiO2 whu.edu.cn
increases and that of ZnIn2S4 decreases in TiO2@ZnIn2S4, Jiaguo Yu − Laboratory of Solar Fuel, Faculty of Materials
further validating the electron transfer from ZnIn2S4 to TiO2 Science and Chemistry, China University of Geosciences,
after contact in darkness. Under 365 nm UV light irradiation, the Wuhan 430074, P.R. China; orcid.org/0000-0002-0612-
8633; Email: [email protected]
peaks of Ti 2p and O 1s in TiO2@ZnIn2S4 move toward higher
Eb (Figure 6a,b), while the peaks of Zn 2p, In 3d, and S 2p in Authors
TiO2@ZnIn2S4 shift toward lower Eb (Figure 6c−e). This Jianjun Zhang − Laboratory of Solar Fuel, Faculty of Materials
outcome illustrates that electron density decreases in TiO2 and Science and Chemistry, China University of Geosciences,
increases in ZnIn2S4, confirming the transport of photo- Wuhan 430074, P.R. China
generated electrons from TiO2 to ZnIn2S4 driven by the BEF Liuyang Zhang − Laboratory of Solar Fuel, Faculty of Materials
(Figure 6f). Consequently, the XPS and ISIXPS measurements Science and Chemistry, China University of Geosciences,
effectively clarify the electron transfer direction in TiO2@ Wuhan 430074, P.R. China
ZnIn2S4 S-scheme heterojunction under dark conditions and
photoexcitation. Complete contact information is available at:
In conclusion, XPS and ISIXPS, with great sensitivity, are https://pubs.acs.org/10.1021/acs.jpclett.2c02125
powerful means to detect subtle changes of elemental Eb due to
changes in electron density in darkness and under illumination. Notes
Hence, the interactions and electron transfer between two The authors declare no competing financial interest.
substances can be reflected by the changes in elemental Eb. XPS Biographies
and ISIXPS measurements are also universal methods for
monitoring electron transfer in heterojunction photocatalysts.
Apart from ascertaining the electron transfer pathways in S-
scheme heterojunctions, the applications of XPS and ISIXPS can
be extended to other photocatalytic systems, such as dye-
sensitized semiconductors and noble metal-semiconduc-
tors.28,29 Furthermore, current research works using ISIXPS in
S-scheme heterojunctions mainly focus on the electron transfer
direction between RS and OS. The influence of UV−vis light
intensity and the BEF strength on the electron transfer process
between RS and OS have rarely been studied. Hence, further
research works on S-scheme photocatalysts based on ISIXPS can
be conducted in the following aspects:
(1) Reveal the effects of UV−vis light intensity on the electron
transfer in S-scheme heterojunctions. The number of electrons
and holes generated in RS and OS is positively correlated with Jianjun Zhang received his B.S. and Ph.D. degrees in Materials Science
the intensity of UV−vis light. With increasing intensity of UV− from Wuhan University of Technology in 2017 and 2021, respectively.
vis light, more photogenerated electrons are produced and He is now a postdoctoral researcher working in the Laboratory of Solar
transfer from the CB of OS to the VB of RS driven by the BEF. Fuel at China University of Geosciences. His current research focuses

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on the electron transfer mechanisms in heterojunction photocatalysts Ph.D. in Materials Science is from Wuhan University of Technology
and perovskite solar cells. (WUT). His research interests include semiconductor photocatalysis,
photocatalytic hydrogen production, CO2 reduction, perovskite solar
cells, electrocatalysis, and so on. He is Foreign Member of Academia
Europaea (2020), Foreign Fellow of the European Academy of Sciences
(2020), and Fellow of the Royal Society of Chemistry (2015).

■ ACKNOWLEDGMENTS
This work was supported by National Key Research and
Development Program of China (2018YFB1502001), National
Natural Science Foundation of China (51932007,
51961135303, 21871217, U1905215, and 52073223), China
Postdoctoral Science Foundation (2021TQ0311 and
2021M702990), and International Postdoctoral Exchange
Fellowship Program (PC2022051).

Liuyang Zhang received her Bachelor of Science degree (2012) from

Shanghai Jiao Tong University. Subsequently, she received her Ph.D.
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