Review
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Photocatalytic and Photoelectrochemical Systems:
Similarities and Differences
Hao Wu, Hui Ling Tan, Cui Ying Toe, Jason Scott, Lianzhou Wang, Rose Amal,*
and Yun Hau Ng*
Photocatalytic and photoelectrochemical processes are two key systems
in harvesting sunlight for energy and environmental applications. As
both systems are employing photoactive semiconductors as the major
active component, strategies have been formulated to improve the
properties of the semiconductors for better performances. However,
requirements to yield excellent performances are different in these two
distinctive systems. Although there are universal strategies applicable to
improve the performance of photoactive semiconductors, similarities and
differences exist when the semiconductors are to be used differently. Here,
considerations on selected typical factors governing the performances in
photocatalytic and photoelectrochemical systems, even though the same
type of semiconductor is used, are provided. Understanding of the underlying
mechanisms in relation to their photoactivities is of fundamental importance
for rational design of high-performing photoactive materials, which may
serve as a general guideline for the fabrication of good photocatalysts or
photoelectrodes toward sustainable solar fuel generation.
1. Introduction
Over the decades, human activities that require clean and
sustainable energy as well as environmentally friendly
Dr. H. Wu, Dr. H. L. Tan, Dr. C. Y. Toe, Prof. J. Scott, Prof. R. Amal,
Prof. Y. H. Ng
Particles and Catalysis Research Group
School of Chemical Engineering
The University of New South Wales
Sydney, NSW 2052, Australia
E-mail: r.amal@unsw.edu.au; yunhau.ng@cityu.edu.hk
Dr. H. Wu, Prof. Y. H. Ng
School of Energy and Environment
City University of Hong Kong
Kowloon 999077, Hong Kong SAR
Dr. H. L. Tan
Department of Applied Chemistry
Faculty of Engineering
Kyushu University
Nishi-Ku, Fukuoka 8190395, Japan
Prof. L. Wang
School of Chemical Engineering
Australian Institute for Bioengineering and Nanotechnology
The University of Queensland
Queensland 4072, Australia
The ORCID identification number(s) for the author(s) of this article
can be found under https://doi.org/10.1002/adma.201904717.
DOI: 10.1002/adma.201904717
Adv. Mater. 2019, 1904717 1904717 (1 of 21)
remediation for environmental issues
have prompted research interest in solar
energy conversion. With the Sun as the
source, energy captured, generated, con-
verted, and perhaps stored, can be used
for addressing mankind’s challenges
in energy shortage and the depletion of
environmental conditions.[1] Besides solar
photovoltaics, which convert sunlight
into electricity, photoactive semiconduc-
tors capable of producing chemical solar
fuels can be considered as the most ideal
means of converting sunlight into a stor-
able and distributable chemical form. This
could potentially be achieved through
photoactive semiconductor-driven water
splitting to generate hydrogen, carbon
dioxide reduction to produce hydro-
carbon fuels (such as methane, methanol,
formic acid, and ethanol), nitrogen fixa-
tion to synthesize ammonia as a hydrogen
carrier, and so on.[2–9] The onset of rapid
development of photoactive semiconductors for use in energy-
and environment-related applications was triggered by the
discovery of Fujishima and Honda in 1972, where a TiO2 photo-
anode was demonstrated to photoelectrochemically split water
into H2 and O2 molecules under ultraviolet illumination.[10] As
water splitting resembles the photosynthesis process in green
plants, it has greatly motivated researchers worldwide to pursue
clean energy production in greener ways.[11] Based on similar
principles, heterogeneous photocatalytic systems that employ
semiconductor powders suspended in aqueous solution have
also been studied and developed extensively. Both photocatalytic
and photoelectrochemical systems offer advantages and limita-
tions, respectively. For instances, it has always been claimed
that photocatalytic system is the simplest way to harvest sun-
light for chemical redox reactions (e.g., water splitting, organic
degradation, CO2 reduction, and N2 fixation).[6,12–16] While
the photoelectrochemical method has a few other strengths
such as the ease of gaseous product separation as well as the
aide of externally applied voltage to manipulate the reaction
mechanism and kinetics for product selectivity tuning.[17,18] A
comparison of the similarities and differences of photocatalytic
and photoelectrochemical systems is summarized in Table S1
(Supporting Information).
In principle, regardless of system type (either photocatalytic
or photoelectrochemical), there are a number of common pro­
perties that the photoactive semiconductors have to possess in
order to facilitate the redox reactions. Typically, a photoactive
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semiconductor must have a reasonable bandgap for it to be

activated (i.e., photoexcitation) by light absorption.[3,19] Upon Hao Wu received his Bachelor
photoexcitation, electrons will be energized into the conduc- of Chemical Engineering
tion band (CB), leaving vacancies (generally known as holes) in degree from China University
the valence band (VB) of the semiconductor. The photoexcited of Petroleum in 2014 and
electrons can then diffuse to the surface from the semicon- subsequently obtained his
ductor bulk to induce chemical reduction while the oxidative Ph.D. in chemical engineering
holes in the valence band are capable of oxidizing the reactant from the University of New
in contact. Ideally, these electron–hole pairs are consumed for South Wales (UNSW) in
chemi­cal reactions at the semiconductor surface, otherwise they 2019. He is now a post-
would be lost through charge recombination. To allow such doctoral research fellow in
surface redox reactions to occur, the photogenerated electrons the School of Energy and
and holes must fulfill the minimum thermodynamic energies Environment, City University
required for the targeted application. Taking water splitting as of Hong Kong. His research interests are on the design of
an example, the CB of a semiconductor must be located at an p-type and n-type oxide semiconductors for photocatalytic
energy more negative than that of the reduction potential of and photoelectrochemical applications.
water to yield H2 while the VB must be more positive than the
oxidation potential of water to produce O2. With these require- Rose Amal is Australian
ments on band energies for redox reactions (not limited to Laureate Fellow and Scientia
water splitting), it is easy to note the challenges in developing Professor in the School
effective photoactive semiconductors that are energetic for both of Chemical Engineering
chemical reduction and oxidation reactions while keeping the at the University of New
bandgap sufficiently narrow for visible light absorption. In fact, South Wales (UNSW). She
considering that the valence band of oxide semiconductors is has worked in the area of
formed by the highly positive O 2p orbital (+3.0 V vs NHE) particle technology for over
and the reduction potential of water is 0 V versus NHE, it is 20 years with an emphasis
rare to have a single narrow bandgap oxide material that can on fine particle aggregation,
split water.[20] Most of the reported efficient visible light active photocatalysis, and nanopar-
oxide semiconductors (e.g., BiVO4 and WO3) are incapable of ticle synthesis. Her current
producing H2 from water.[21–23] In contrast, perovskite oxides research focuses on designing nanomaterials for solar to
are another group of promising photocatalytic materials due chemical energy conversion applications (including photo-
to the flexibility in their bandgap and band edge tuning.[24,25] catalysis for water and air purification, water splitting, and
Nonoxide photoactive semiconductors such as nitrides[26,27] CO2 reduction) and engineering systems for solar-induced
and sulfides[28–30] may offer greater reducing capability as they processes.
possess a more negatively located CB. Although equipped with
a high reducing potential, these nonoxide semiconductors may
have a tendency to suffer from photocorrosion and thus result Yun Hau Ng received his
in instability over long-term illumination.[31–34] On combining Ph.D. from Osaka University,
two photoactive semiconductors with respective strengths in Japan, in 2009. After a brief
either their reducing or oxidizing potential, maximized redox research visit to the Radiation
potentials by capitalizing the energetic VB of oxides and the Laboratory at the University of
energetic CB of nonoxides can be achieved through the con- Notre Dame (USA), he joined
struction of Z-scheme photocatalytic or bias-free photoelectro- the ARC Centre of Excellence
chemical systems. Readers are recommended to the excellent for Functional Materials at
works that provided detailed mechanistic understanding of the UNSW with the Australian
Z-scheme photocatalytic and bias-free photoelectrochemical Postdoctoral Fellowship
systems included here.[35–39] (APD). He became a lecturer
The abovementioned common properties (including (2014) and senior lecturer
bandgap, band energies, surface redox reactions, and so on) are (2016) at the School of Chemical Engineering, UNSW. He
generic to photoactive semiconductors regardless of the ways is currently an associate professor at the School of Energy
they are used (photocatalytic or photoelectrochemical systems). and Environment, City University of Hong Kong. His
There are, therefore, universal strategies applicable to most research is focused on the development of novel photoac-
photoactive semiconductors to improve those properties. These tive semiconductors for sunlight energy conversion.
include bandgap tuning to increase light absorption (in most
cases it is bandgap narrowing, but it can be bandgap widening
when it comes to quantum dot development), band energy as loading a cocatalyst to improve surface charge transport,
modulation to adjust redox capabilities, and photocharge trans- doping of foreign atoms into the regular crystal lattice of a
port enhancement to increase charge utilization. Experimen- semiconductor to introduce impurity energy levels that essen-
tally, these strategies involve some common methods such tially change the bandgap and band energy, and nanotexturing

Adv. Mater. 2019, 1904717 1904717 (2 of 21) © 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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Figure 1. a) Schematic illustration and b) requirement of redox potential for photoinduced oxidation and reduction reactions (in this case, water
splitting) using a photoactive semiconductor, in which (i) photon absorption, (ii) charge separation and transfer, and (iii) surface chemical reactions
are the three main components. a,b) Reproduced with permission.[66] Copyright 2010, Elsevier B.V.
the semiconductor to increase the surface area.[40–49] A great
number of comprehensive reviews on these topics, ranging
from design and fabrication of materials to material characteri-
zations and reactor design, have been produced over the last
two decades.[49–65] Despite being applicable to various groups of
photoactive semiconductors, these synthetic, modification, and
design strategies may impose different levels of effectiveness or
sometimes even result in conflicting outcomes when the same
photoactive semiconductor is employed in different systems:
photocatalytic or photoelectrochemical systems.
Photocatalytic system usually (not all, but the majority)
involves development of semiconductor powder that is sus-
pended in an aqueous solution; photoelectrochemical system
requires utilization of photoactive thin film(s), which is
obtained either through direct thin film synthesis or by immo-
bilizing the semiconductor powder onto a supporting electrode
surface, in the presence of an electrolyte (Figure 1).[66] Meth-
odologies in designing and fabricating powdered or thin-film
semiconductors have been developed to control a vast variety of
properties including shape, crystallinity, multicomponent com-
position etc.[67–71] In a photocatalytic system, the semiconductor
powder is homogeneously suspended in an aqueous medium
that restricts effective light penetration through the medium
to reach the semiconductor. The need of the semiconductor
to be water-miscible also necessitates the presence of certain
surface functionalities on the material. These factors, which
govern photocatalytic activity, are different to those required in
a photoelectrochemical system, albeit the same semiconductor
is employed. Close and high quality contact between semi-
conductor and the charge collecting substrate (typically trans-
parent conducting substrate) entails effective charge transfer
to achieve excellent photoelectrochemical activities. Such a
requirement is irrelevant to photocatalytic system. Therefore,
although there are generic strategies to improve the perfor-
mance of photoactive semiconductors as documented in the
literature, there remain similarities and differences imposed
by the same strategies depending on the way the semiconduc-
tors are to be used. Discussions in this regard are seldom in the
literature. Although not being exhaustive, this didactic review
aims to discuss and provide considerations on typical factors,
which govern semiconductor performance in photocatalytic
Adv. Mater. 2019, 1904717 1904717 (3 of 21)
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and photoelectrochemical systems, on the basis that same
semiconductor is used. The weighting of certain factors can
be greatly different when the semiconductor is employed in
a different way. Section 2 of this paper covers the similarities
and differences in designing highly efficient photocatalytic
and photoelectrochemical systems with a focus on the typical
factors that govern the performance including particle size,
crystallinity, dimensionality, composite structure, and configu-
rations. The limitations and potential solutions of each system
(photocatalytic or photoelectrochemical systems) are discussed
in Section 3 in conjunction with the perspective on future strat-
egies. Understanding of the underlying mechanisms in rela-
tion to their photoactivities is of fundamental importance for
rational material design to deliver an optimum structure, and
may serve as a general guideline for fabricating highly effective
photocatalysts or photoelectrodes.
2. Similarities and Differences
Efforts in improving the performance of photoactive semi-
conductors have been explored comprehensively that are
mainly directed at improving light absorption (e.g., bandgap
engineering and doping), redox potentials (e.g., band energy
engineering), and bulk and surface charge carrier dynamics
(e.g., crystal facet engineering, heterostructure construc-
tion, morphological control, and addition of cocatalyst and so
on).[72–81] The state-of-the-art photoactive semiconductors for
photocatalytic and photoelectrochemical water splitting are
summarized in Tables S2 and S3 (Supporting Information),
respectively. In this section, the similarities and differences of
the factors governing photocatalytic and photoelectrochemical
systems will be discussed.
2.1. Particle Size and Crystallinity
It is generally perceived that a larger specific surface area
provides augmented active sites for reactant adsorption and
promotes charge transfer across the interfaces, which include
the solid–solid and solid-liquid boundaries. The solid–solid
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Figure 2. a,b) TEM images of ZnO nanorods with controlled aspect ratio (i.e., size) and c,d) SEM images of Cu2O cubes with different sizes. a,b) Repro-
duced with permission.[83] Copyright 2004, Royal Society of Chemistry. c,d) Reproduced with permission.[84] Copyright 2016, American Chemical Society.
interfaces describe the interparticle contacts within single
or multicomponent particulate semiconductors, whereas,
the solid–liquid interfaces represent the boundaries between
the semiconductor and the reactants (i.e., charge donor and
acceptor) in the aqueous phase. The positive correlation between
the specific surface area of photocatalyst/photoelectrode and
their photoactivities has been widely documented. Nanosized
materials with large specific surface area have therefore been
popularly employed in this field of research (Figure 2).[82–84]
The photoactivities of oxide semiconductors have generally
been restricted by their short carrier lifetimes and low charge
mobility. These can be addressed by nanostructuring, in which
shorter charge transfer pathways are provided to facilitate
carrier diffusion to the interfaces to achieve higher solar energy
conversion efficiency.[46,85] In a photoelectrochemical system,
the surface area of a thin-film photoelectrode can be enlarged
by inducing microporosity in the film via sacrificial template
deposition, by surface roughening and texturing (Figure 3), and
by nanostructuring (e.g., nanowires and nanorods, which will
be covered in Section 2.2).[86–88]
Aside from the advantages discussed above, nanostruc-
turing is also helpful in enhancing light absorption. In parti­
cular, nanostructured surfaces are useful as antireflection and
increased light scattering to assist in increasing the optical
path length of incident irradiation, as illustrated in Figure 4.[49]
Note that the light distribution induced by nanostructuring
is single direction (typically horizontal) for photoelectrodes
and 3D for a particle suspension. Wang and co-workers dem-
onstrated the construction of internal spherical porosity in
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their photoelectrode boosted light scattering and resulted in
improved photoactivity.[89] Presence of a periodic nanostructure
(e.g., opal- or inverse opal-nanostructured thin films) has also
been demonstrated helpful in light trapping of a specific wave-
length useful for photoactivity enhancement.[90,91]
The positive effects of nanoscaling have been shown as
predominant in most studies. However, the different effects
of nanostructuring observed in photocatalytic and photoelec-
trochemical systems should be taken into consideration for
efficient catalyst configuration. Although the specific sur-
face area and light absorption ability of a semiconductor can
be improved through nanoscaling, charge separation may be
adversely affected. Typically, the charge separation in a semi-
conductor is assisted by the built-in electric field induced by the
space charge layer present near the semiconductor surface. The
formation of space charge layer is caused by the charge equi-
libration between the semiconductor and the other phases in
contact, detailed of which can be found elsewhere.[92] Such a
space charge layer thickness is dependent on the particle size
and is nearly negligible in nanoparticles.[93] Given the absence
of the space charge layer, that is, no interior electric field, the
charge separation ability of a semiconductor is compromised
when it is being downsized to nanoscale.
Crystallinity is another important factor that governs the
photoactivity of a semiconductor as it critically affects the
intrinsic charge separation and transport of the material. A
higher crystallinity has fewer recombination centers to promote
more photoexcited electron–hole pairs to diffuse from the semi-
conductor bulk to surface to initiate redox reactions. An ideal
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Figure 3. a–d) AFM images of TiO2 thin films roughened by Bi2WO6 deposition with different loadings: a) Bi2WO6-0%, b) Bi2WO6-1.5%, c) Bi2WO6-3%,
and d) Bi2WO6-5%. a–d) Reproduced with permission.[86] Copyright 2011, American Chemical Society.

material is one that possesses both a high degree of crystallinity
and a high specific surface area. However, the surface area of
a semiconductor is generally increased at the expense of its
crystallinity or vice versa. The enriched surface defect density
in small particles generally reduces the crystallinity of the mate-
rials. On the other hand, postsynthesis treatment of a semicon-
ductor by heating or annealing at an elevated temperature or
pressure either in gas phase (e.g., calcination in air) or liquid
phase (e.g., hydrothermal treatment) is typically conducted in
order to improve the crystallinity of the material. Such a post-heat
treatment, however, always results in aggregation/sintering/
agglomeration of the particles. A trade-off between crystallinity
and surface area is therefore needed for optimal performance.
Despite this, Kato and co-workers demonstrated the feasibility
to fabricate NaTaO3 nanoparticles with high crystallinity merely
via lanthanum doping without the need of subsequent heat
treatment.[94] With improved crystallinity, the particle size of the
La-doped NaTaO3 powder (0.1–0.7 µm) was smaller than that
of the nondoped NaTaO3 powder (2–3 µm). However, such a
doping strategy is not universally applicable to all semiconduc-
tors as a means for crystallinity improvement. Most studies in
the literature continue to experience the compromise between
crystallinity and surface area (particle size).[92,95–97]
Many studies have reported enhanced photocatalytic and
photoelectrochemical performances achieved with the use of
nanoparticles or nanostructuring. The results are robust and
reproducible in many laboratories. Decoupling the factors
contributing to enhanced activities is challenging and rarely

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Figure 4. a–c) Light distribution in flat films (a), rough films (b), and
particle suspensions (c). A: surface area; d: film or particle thickness; α−1:
optical penetration depth. Short arrows show scattered or reflected light.
a–c) Reproduced with permission.[49] Copyright 2013, Royal Society of
Chemistry.
quantified. There are reports that showed contrary effects
of nanosizing, particularly in the photocatalytic system.[82,98]
Owing to the poor charge separation arising from poor crys-
tallinity and the absence of space charge layer in small parti-
cles, the O2 evolution performances on WO3 and BiVO4 were
shown to be deteriorating with decreasing particle sizes. These
downsides of nanoparticles, however, are suppressed in the
photoelectrochemical system due to the different charge sepa-
ration mechanisms involved. An externally applied bias can
be used to promote shuttling of majority carriers from the
photoilluminated electrode to the counter electrode. Addition-
ally, even without an external bias as in the case of zero-bias
photoelectrochemical setups, careful control of the photo-
electrode film thickness (i.e., thickness of the semiconductor
powder immobilized on the conducting substrate in the case
a particulate photoelectrode) in the range of minority diffusion
length enables effective charge separation in the absence of
space charge layer. This is because film thickness smaller than
the minority diffusion length allows efficient minority carrier
photogeneration throughout the electrode, in which the carriers
could migrate to the photoelectrode/electrolyte interface. Mean-
while, the presence of an external circuit provides a continuous
majority carrier transport pathway.[99]
Heat treatment of the photoelectrode has been regu-
larly practiced to improve the photoelectrochemical per-
formance.[100,101] Although crystallinity can be improved
Figure 5. SEM images of photoactive semiconductors with different dimensions: a) 0D TiO2 nanoparticles film, b) 1D ZnO nanorod film,
c) 2D vertically aligned SnS2 nanosheet film, and d) 3D highly ordered BiVO4 film. a) Reproduced with permission.[109] Copyright 2009, Royal Society of
Chemistry. b) Reproduced with permission.[107] Copyright 2015, Royal Society of Chemistry. c) Reproduced with permission.[108] Copyright 2017, Royal
Society of Chemistry. d) Reproduced with permission.[106] Copyright 2013, Wiley-VCH.
Adv. Mater. 2019, 1904717 1904717 (6 of 21)
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(depending on the annealing temperature), another main
function of the heat treatment is to bettering the adhesive
strength or allow intimate contact between the immobilized
semiconductor and the charge-collecting substrate. While the
charge separation and transport within a photoelectrode can
be manipulated by the applied bias and the film thickness, the
charge transfer ability of the majority carries at the semicon-
ductor/substrate interface is crucial to account for the charge
transfer across the external circuit. The quality and intimacy of
the contact between the semiconductor and the substrate has
therefore become a real focal point in the community (which
is discussed further in the ensuing section). This aspect is not
a consideration in the powder-suspension of a photocatalytic
system.
2.2. Shape, Structure, and Architecture of a Single-Component
Semiconductor
With the advances in materials science, photoactive semicon-
ductors can now be conveniently designed and tailor-made into
various sizes, shapes, and architectures according to the needs
of the photoreaction and the photoreactor design. In general,
photoactive semiconductors are designed toward nanoscale
or submicron scale to maximize their solar energy conversion
efficiency for a number of valid justifications as described in
Section 2.1, although the ultimate ideal material is yet to be
realized.[9,93,102–105] For both photocatalysts and photoelec-
trodes, the photoactive semiconductors can be synthesized in
the form of 0 dimension (0D), 1D, 2D, and 3D with various
shapes (Figure 5).[77,105–113] In a photocatalytic system where
the photocatalyst powder is homogeneously suspended in an
aqueous solution, once the incident light reaches the particle
surfaces, light scattering happens on all sides and thus length-
ening the light penetration path and improving light absorption
(Figure 6).[114] For every freely suspended photocatalyst particle,
the photogenerated charge carriers only need to migrate from
the bulk to the particle–liquid surface for conducting redox
reactions. The charge diffusion lengths are therefore relatively
shorter compared to other system configurations. There is an
increasing number of studies reporting the development of
photocatalytic thin films in which the powdered photocatalyst
is coated on a nonconducting glass for nonsuspension type
photocatalytic water splitting.[115–118] For those photocatalytic
thin films, the requirements for the photoactive semiconductor
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Figure 6. Light scattering/trapping and charge transport in nanostructures of single materials as a suspended photocatalyst or a photoelectrode:
a) 0D nanocrystals, b) 1D nanostructures, c) 2D nanosheets, and d) 3D nanostructures. a–d) Reproduced with permission.[114] Copyright 2015, Royal
Society of Chemistry.
are even higher and more stringent as the light scattering
pheno­menon is less significant and there is no applied voltage
provided to drive the redox reactions.[117] 0D particles are ideal
for suspension-type photocatalytic reactions. In contrast, when
0D particles are immobilized on a conducting substrate for a
photoelectrochemical reaction, the electron migration behavior
is different and negatively impacts the overall performance.
Taking the photoanode as an example, the photogenerated
electrons on 0D particles have to shuttle through countless
interparticle interfaces before reaching the charge collecting
substrate.[21] Despite being porous (an assembly of 0D particles
always result in the presence of porosity) with a larger specific
surface area, the probability of encountering charge traps–
detraps across the interparticle boundaries, charge recom-
bination and back reactions is also higher for 0D particles
assembled into photoelectrodes.[49]
A 1D photoactive semiconductor immobilized or directly
grown on the charge collecting substrate offers potential solu-
tions to the poor charge transport encountered by 0D materials
in the photoelectrode configuration. Studies indicate that the
longitudinal direction of 1D crystalline nanostructures can serve
as a preferential pathway for electron migration.[119] Nanotubes,
nanorods, nanowires, nanofibers, and nanoneedles are among
the typical 1D nanostructured photoactive semiconductors
that have been grown on substrates for photoelectrochemical
applications.[120–125] Grimes and co-workers demonstrated the
presence of less-localized charge carriers in a 1D nanostruc-
ture when compared to the same material in a 0D form which
favored solar energy conversion applications.[126] 1D nanostruc-
tures can also enable modulation of the crystal facet structure
at the material surface, which can influence performance. For
instance, Wu and co-workers examined 1D TiO2 nanobelts in
a suspension-type photocatalytic reaction. They found that
TiO2 nanobelts with a preferentially exposed (101) facet pro-
moted superoxide anion generation due to the interaction
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with preferentially adsorbed O2.[127] Based on the dimensional
engineering of photoactive semiconductors, crystal facet engi-
neering is another aspect that can be tuned towards targeted
reactions (to be discussed in following part of this section).
2D photoactive semiconductors are an emerging class of sheet-
like photocatalysts for freestanding use in suspension.[60,110]
Among 2D photoactive semiconductors, graphitic carbon
nitride (g-C3N4) nanosheets have attracted great attention from
the research community as they demonstrate desirable prop-
erties as an efficient photocatalyst for a number of important
redox reactions.[128–130] Predominantly attributed to its large
exposed surface area with extreme thinness, 2D photoactive
semiconductors have a large solid–liquid interface for surface
chemical reactions, which further empowers the short dif-
fusion length for photoexcited charges to reach the surface.
Additionally, the large exposed surface area enables supplemen-
tary chemical functionalization of the basal planes to modulate
its surface chemistry (such as hydrophilicity). Ultrathin defec-
tive 2D TiO2 nanosheet has shown to exhibit good photo­catalytic
N2 reduction performance due to the strong chemisorption
toward N2 molecules on the oxygen defect sites.[131] On top of
that, a recent review article has also provided a thorough evalu-
ation of 2D-based materials utilized for solar-driven COx con-
version, in which photoactivity and selectivity optimization
strategies were comprehensively reviewed.[60] A 2D structure
can be used as a scaffold to support the formation of composite
materials when a heterojunction with another semiconductor
is desired. For example, due to the feasibility in constructing
heterojunction composite materials, 2D g-C3N4 has been widely
used as the platform to prepare type II and Z-scheme hetero-
structures in suspension-type photocatalytic systems.[132,133] In
a photoelectrochemical configuration, if the 2D nanosheets can
be vertically aligned on the transparent conducting electrode,
they also offer light trapping and scattering effects that consid-
erably increase the incident light path length. Ultrathin In2S3
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Figure 7. TEM images of photoactive semiconductors with 3D, highly ordered structures (3DOM): a) TiO2–SiO2 composite, b) Fe2O3–BiVO4 composite,
and c) pure TiO2 semiconductor. a) Reproduced with permission.[136] Copyright 2016, Wiley-CH. b) Reproduced with permission.[137] Copyright 2017,
Elsevier B.V. c) Reproduced with permission.[138] Copyright 2017, Cell Press.
nanosheets and SnS2 nanosheets are the two examples of 2D
photoactive semiconductors vertically aligned on an electrode
reported for photoelectrochemical water splitting.[134,135]
3D-ordered meso/macroporous (3DOM) photoactive semi-
conductors are another class of materials receiving attention
owing to their excellent photocatalytic activity (Figure 7).[136–138]
Although not all 3D semiconductors are porous or highly
ordered, in this section we focus only on 3DOM semicon-
ductors with a hierarchical structure due to their interesting
structure, which influences light trapping and electron
transportation. Nonporous or nonordered 3D photoactive
semiconductors in many cases can be regarded as joined or
aggregated particles of 0D, 1D, or 2D materials, and therefore are
not discussed here. 3DOM photoactive semiconductors are
typically prepared through a templating method using sacri-
ficial building blocks such as self-assembled polymer spheres
and block copolymers.[106,139] 3DOM photoactive semicon-
ductors, when carefully designed, can demonstrate unique
optical features of photonic crystals such as waveguiding, light
trapping, and scattering.[140] These features cannot be observed
in disordered 3D structures. The excellent photocatalytic activi-
ties of 3DOM photocatalysts are primarily attributed to their
large surface area, occasionally additional evidence of enhanced
light absorption resulting from scattering phenomena could be
observed. However, as the internal wall of 3DOM photocatalysts
are highly crystalline and extremely thin, typically in the range
of a few nanometers, it is anticipated that the electron diffusion
length, charge mobility, and charge lifetimes will be different
compared to bulk materials. A higher surface area is likely to
be one of the key reasons for good performance although the
bearing of charge transport in 3DOM photocatalysts is largely
underexplored at this time. Although 3DOM photocatalysts
have a demonstrated potential for photocatalytic systems, their
usefulness in the photoelectrochemical domain is another
aspect yet to be carefully investigated. Unless the 3DOM semi-
conductor can be directly grown on the conducting substrate
(without having the presynthesized particulate as intermediate),
contact between the 3DOM semiconductor and the conducting
substrate is expected to be a considerable weakness toward cap-
italizing on the advantageous properties of 3DOM materials.
At present, the vast majority of 3DOM semiconductors are pro-
duced in a powder form. The powder 3DOM semiconductors
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can be loaded or coated onto the conducting substrate when
used in a photoelectrochemical array. The pointy edges of the
3DOM structure will be, in principle, the contact points with
the conducting electrode substrate. Consequently, the contact
area between the 3DOM material and the electrode substrate
will be limited. The multifold enhancement of photoactivities in
a 3DOM structure, as compared to its bulk counterpart, within
a suspension-type photocatalytic system cannot be achieved in a
photoelectrochemical system (unless a high external voltage is
provided). The unique features and their beneficial effects (light
trapping, scattering, rapid intrinsic charge extraction) may be
compromised by the limited contact with the electrode sub-
strate. The requirements for achieving good photocatalytic and/
or photoelectrochemical performance again vary based on the
operating conditions.
Crystal facet engineering can be regarded as a subset of
nanostructure engineering with the specific aim to promote or
prohibit the anisotropic growth of a crystal in a certain direc-
tion. The crystal facets of photoactive semiconductors have
been studied since the early 2000s where Ohno and co-workers
experimentally demonstrated the reduction and oxidation
sites on a TiO2 particle were located on different facets.[141]
As there are different atomic coordinations and configura-
tions associated with different facets, the preferential expo-
sure of a specific crystal facet of a semiconductor can exhibit
distinct optical and electronic properties. Since the work by
Ohno and co-workers, photoactive semiconductors with con-
trolled crystal facet orientation have garnered significant
interest and are used as a tool to manipulate charge transfer
and separation processes, predominantly in suspension-based
photocatalytic systems (Figure 8a).[142–144] Comparatively, crystal
facet-engineered photo­electrodes have been less studied com-
pared to their powder counterparts due to the greater chal-
lenges (Figure 8b).[145–147] In the case of photoelectrodes, there
are crystal facets that are exposed to the aqueous medium for
redox reactions (the same as for crystal faceted powders) and
crystal facets which are in contact with the substrate. The inter-
face between the semiconductor and the electrode substrate is
the critical region where charge transfer occurs for delivery to
the counter electrode. This interface does not exist for photo-
catalyst particles. Considering a photoanode, for example, at
the semiconductor–substrate interface, when the work function
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Figure 8. a) SEM images of crystal facet-engineered powder photocatalysts: TiO2, BiVO4, and Cu2O. b) SEM images of crystal facet-engineered
photoelectrodes: TiO2, BiVO4, and Cu2O. Image for TiO2 in (a): Reproduced with permission.[144] Copyright 2008, Springer Nature. Image for BiVO4 in
(a): Reproduced with permission.[142] Copyright 2016, American Chemical Society. Image for Cu2O in (a): Reproduced with permission.[143] Copyright 2018,
Wiley-VCH. Image for TiO2 in (b): Reproduced with permission.[147] Copyright 2011, Royal Society of Chemistry. Image for BiVO4 in (b): Reproduced with
permission.[146] Copyright 2017, Wiley-VCH. Image for Cu2O in (b): Reproduced with permission.[145] Copyright 2011, Springer Nature.

of the semiconductor is larger than the conductive substrate,
downward band bending will happen and photogenerated
electrons can flow from the semiconductor to the substrate.
When the work function of the substrate is larger, upward band
bending will occur (Schottky barrier) and photoelectrons in the
CB of the semiconductor cannot be transferred and activity
ceases. Therefore, crystal facet engineering at the interface of
the semiconductor and the conductive substrate can be used to
tailor the work function relationship between the two compo-
nents and influence charge transfer. Crystal facet-engineered
photoelectrodes have more criteria to meet than particle-based
suspensions as there are two key interfaces involved: the solid–
solid interface (semiconductor–substrate) and the solid–liquid
interface (semiconductor-electrolyte/aqueous reactant).
2.3. Multicomponent Composites and Their Configuration
As discussed earlier, in addition to the inadequate charge trans-
port properties (low charge mobility, short lifetime, slow sur-
face kinetics), a single photoactive semiconductor also faces the
challenge of meeting the needs for large redox potentials with
a sufficiently narrow bandgap for visible light absorption. Cou-
pling two or more components into a photoactive composite
may address some of these drawbacks by utilizing the strengths
of individual semiconductors. The secondary, or additional,
component can be another photoactive semiconductor (e.g.,
to form a plasmonic composite, Type I, Type II, or Z-scheme
configuration), cocatalyst (to promote surface kinetics or to
serve as a passive layer), or a metallic/nonmetallic conductor
(to boost electron transfer).[148–156] In brief, the multicompo-
nent photoactive composites offer photocatalytic benefits one or
more of the following aspects: 1) extending the light absorption
spectrum; 2) promoting charge separation; 3) minimizing
charge losses through recombination; and 4) passivating
photocorrosion. These aspects will not be further discussed
here as excellent reviews on the functions of multicomponent
photoactive composites and the roles of individual components
are otherwise available.[157–161] Here, the discussion will focus
on those aspects to be considered when the multicomponent
photoactive composites are to be used in either photocatalytic
or photoelectrochemical systems.
Typically, the deposition of cocatalysts (e.g., metal or metal
oxide) on photocatalysts could exhibit both enhanced photo­
catalytic and photoelectrochemical activity if appropriate
cocatalyst is employed (Figure 9a,b). The type of cocatalysts
strongly relies on the specific applications; for instance, Pt (an
excellent electron sink) for hydrogen evolution reaction,[162,163]
CoPi for oxygen evolution reaction,[164,165] and Cu- or Ni-based
cocatalysts for CO2 reduction reaction.[157] Owing to the
distinct nature of charge transfer in photocatalytic and photo­
electrochemical systems, the design of cocatalyst loaded photo­
catalysts could be very different from cocatalyst deposited
photoelectrodes. As illustrated in Figure 9a,b, oxidation and
reduction cocatalysts could both be loaded on the same photo-
catalyst (either n- or p-type) to be used in a suspension system.
For example, deposition of dual cocatalysts (Pt as hydrogen
evolution catalyst and PdS as oxidation cocatalyst) has shown
to significantly enhance the overall hydrogen production of
CdS photocatalyst.[166] On the other hand, these cocatalysts
must be deposited separately on n- and p-type photocatalysts
as the photoanode (for oxidation) and photocathode (for reduc-
tion), respectively, in a photoelectrochemical system. Despite
the difference, surface chemistry of the cocatalyst that acts as
the reaction active site and its interaction with the photocata-
lyst play the important roles in facilitating both photocatalytic
and photoelectrochemical systems. A comprehensive review by
Yang et al. has described and compared the differences in the
role of co-catalyst for photocatalytic and photoelectrochemical
systems.[41]

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Figure 9. Typical structures of multicomponent composites for photocatalytic and photoelectrochemical systems. a,b) Cocatalyst deposition for
powdered photocatalyst (a) and thin-film photoelectrodes (b). c) Core–shell structure for powdered photocatalyst, d) core–shell structure and
passivation layer of photoelectrodes.

Core–shell architecture is a popular approach when con-
structing composite materials, especially in powdered photo­
catalysts (Figure 10).[167–169] When a semiconductor particle
is coated with a conformal layer of an additional component,
a core–shell structure is formed. The distinct surface chemical
composition introduced by the core component can also invoke
the four benefits mentioned above. For instance, encapsulating
an unstable photoactive semiconductor (such as Cu2O) within
another semiconductor shell can enhance its stability against
photocorrosion (i.e., photoinduced oxidative or reductive
dissolution).[170] Apart from having the photocatalyst as the core
structure, coating the photoactive semiconductor as the outer
layer appears to be beneficial under certain circumstances, as
illustrated in Figure 9c. By designing different configuration
of the core and shell components, the equilibrium Fermi
energy level can be tailored such that the electrons or holes can
be stored in the core while charge transfer between the shell
layer and the aqueous medium is promoted. This separation
of photoexcited charges based on the band energy alignment
prolongs charge lifetime and is potentially beneficial to the
overall photocatalytic performance.[171] Additionally, tiny mag-
netic particles encapsulated within a semiconductor shell have
proven to bring advantages for suspension-type photocatalytic
systems, particularly in wastewater treatment applications.
Although not altering any of the optical or electronic properties
of the photoactive semiconductor, the presence of a magnetic
core facilitates photocatalyst recovery upon completing the
reaction.[172–174]
In a photoelectrochemical configuration, multicomponent
photoactive composites are constructed in a core–shell structure
for a similar, yet slightly different, reason (Figure 11).[175,176] To
construct a core–shell-structured photoelectrode, usually the
shell semiconductor suffers from a shorter minority charge
diffusion length than the optical penetration path. Despite the

Figure 10. TEM images of core–shell-structured nanoparticles: a) CdS–ZnS, b) Au–Cu2O, and c) crystalline TiO2–amorphous TiO2. a) Reproduced
with permission.[167] Copyright 2014, Royal Society of Chemistry. b) Reproduced with permission.[168] Copyright 2011, American Chemical Society.
c) Reproduced with permission.[169] Copyright 2016, Wiley-VCH.

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Figure 11. Core–shell nanostructured photoelectrode directly grown on a thin film. a,b) TEM and HRTEM images of ZnO nanorod (core)–CdS (shell),
c,d) TEM and HRTEM images of TiS2 nanorod (core)–Fe2O3 (shell). a,b) Reproduced with permission.[175] Copyright 2015, Royal Society of Chemistry.
c,d) Reproduced with permission.[176] Copyright 2011, American Chemical Society.

entire photoelectrode being able to absorb the incident light
due to the sufficient optical penetration length, the extremely
short charge diffusion length is a bottleneck for charge con-
sumption and, in turn, photoactivity. Thus, charge extraction
at the photogeneration site can be useful for transporting the
photoexcited charges in a secondary component while enabling
maximum light absorbance.[3,177] Taking Fe2O3 as an example of
a photoactive semiconductor with short charge diffusion length,
fabricating a vertically aligned core–shell TiSi–Fe2O3 structure
on a photoelectrode greatly enhanced the photocurrent com-
pared with a bare Fe2O3 photoelectrode. Upon photoexcitation,
the charges in Fe2O3 do not have to travel (actually it is impos-
sible to) throughout the entire nanorod/nanowire array to reach
the conductive substrate. As the 1D core TiSi is highly con-
ductive, it provides a “highway” and extraction point to allow
charge transfer from the excited Fe2O3 to occur. The transferred
electrons are subsequently shuttled along the longitudinal
direction to the substrate.[176] For the purpose of passivating the
photoinduced dissolution of an unstable semicoductor, core–
shell design may not be the only strategy whereby the more
commonly adopted and facile layer-by-layer coating approach
may suffice (Figure 9d).
In addition to the widely established motivation in forming
a heterojunction composite for extended light absorption and
better charge separation/transfer, introducing a secondary com-
ponent to a thin-film photoelectrode can play a significant role
in passivating the surface of the underlying semiconductors.
Unlike core–shell particles that are relatively difficult to form
shell layers with complete coverage, the layer-by-layer deposition
of secondary components on top of the photoactive semicon-
ductor thin film can be achieved using various techniques, such
as high-cost physical vapor deposition (PVD), chemical vapor
deposition (CVD), atomic layer deposition (ALD), or low-cost
electrodeposition, photoelectrodeposition, and solution-based
coating methods. For example, a relatively inert metal oxide thin
layer (e.g., Ga2O3 and Al2O3) has been deposited on an n-type
hematite photoanode using chemical bath deposition.[178,179]
An atom-thick Al:ZnO layer was deposited on a p-type Cu2O
layer to improve photocathode photostability.[145] Photocorro-
sion pathways of Cu2O changes with the addition of externally
applied bias in a photoelectrochemical system when compared
to photocatalytic system that is mainly governed by intrinsic
charge properties of Cu2O.[180] Forming a solid–solid interface to
replace the solid–liquid interface (i.e., hematite–water interface)

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has been a guiding principle used by researchers to minimize
surface recombination or surface chemical reaction of the pro-
tected semiconductor. In brief, the mechanisms involved in the
photostability improvement can be related to better catalysis,
higher photovoltage, and/or reduced recombination, with each
mechanism interrelated. The exact roles of the passivation layer
in thin-film photoelectrodes are complicated; further reading
is available in Wang’s recent review article.[52] The “passivation
layer” constructed in the form of a buried junction can also
reduce surface states that suppress recombination and catalyze
electron transfer. When considering charge transfer promotion
in a multicomponent photoactive electrode, energetic matching
is another important factor. If the energetic mismatch is too
significant, the collected excited charges may not have a suffi-
cient driving force for the specific redox reaction. For example,
p-type Cu2O can be coupled with an n-type ZnS or Ga2O3 layer
for photoelectrochemical water reduction.[170,171] Although both
the ZnS and Ga2O3 layers can improve the HER, the significant
mismatch in band energy in Cu2O/ZnS is less favorable for the
reaction. Another important aspect to be considered during
the design of multicomponent photoelectrode is the illumina-
tion direction (in particular, electrodes with glass/transparent
substrate). It has been reported that front photoelectrode illumi-
nation could yield a very distinct performance when compared
to back illumination using the exact same electrode (Figure 9d).
Unlike photocatalytic suspension system where light could be
assumed to homogenously irradiated on every surface of the
particles via mixing, the direction of light could determine the
photoexcitation efficiency of each layer of a photoelectrode.
Therefore, although construction of a multicomponent photo­
active composite is effective in improving overall photoactivities
in photocatalytic and photoelectrochemical systems, the consid-
erations driving material design can differ.
2.4. Characterization and Evaluation of Photocatalyst and
Photoelectrode
Given that the key component of a photocatalyst and a photo-
electrode is essentially the same material (with variations in
terms of size, shape, crystal structure, surface chemistry, and so
on), the characterization techniques for both photocatalyst and
photoelectrodes largely overlap. This includes the general char-
acterization of physical properties, optical bandgap, absolute
band energy positions, and dynamics of the photogenerated
electrons and holes (such as diffusion length, mobility, lifetime,
charge recombination and transfer rate).
To evaluate the bandgap energy of a photoactive semicon-
ductor, optical methods based on spectroscopies are the most
convenient and straightforward way despite the availability of
other nonspectroscopic techniques, such as the Hall constant
and photoconductivity measurements. Among all optical spec-
troscopic techniques, ultraviolet–visible diffuse reflectance spec-
troscopy (UV–vis DRS) is the most frequently used for both pho-
toelectrodes and powdered photocatalysts. Conventional plots
of reflectance or absorbance against wavelength can be used to
determine the absorption/reflectance edge, which resembles
the energy level that separates the CB and VB. Another optical
tool that complements UV–vis DRS is surface photovoltage
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spectroscopy (SPS). SPS measures the surface potential
changes as a function of incident photon energy. Redistribution
of the free charges photogenerated in a semiconductor triggers
the surface photovoltage (SPV). Attributed to the Franz–Keldysh
effect and excitation of trapped states, SPV can serve only as
estimation due to the broad SPV signal onset.[181,182]
The absolute positions of the CB and VB are one of the
governing factors defining the redox capability of a photoactive
semiconductor. While their absolute values can be theoreti-
cally predicted using density functional theory, the direct use of
experimental approaches has become more attractive. Some of
the commonly used experimental techniques based on the flat
band potential (Efb) measurement include a) capacitance meas-
urement using the Mott–Schottky equations, b) photocurrent
onset determination—the potential at which the photocurrent
appears corresponds to the Efb of the semiconductor; c) open-
circuit potential (Voc) measurement in which the constant
potential observed at a high illumination intensity is regarded
as the Efb of the semiconductor.[183] X-ray photoelectron spec-
troscopy (XPS) and ultraviolet photoelectron spectroscopy
(UPS) are two other spectroscopic techniques used to determine
the VB position in a semiconductor. Typically, the VB potential
is evaluated from the leading edge of the photoemission spec-
trum that is close to 0 eV binding energy. While a hybrid exper-
imental–theoretical approach known as Kraut method can be
used, the most commonly employed technique to estimate VB
potential is via the intersection point between the background
line and the regression line fitted to the linear region of the
XPS/UPS leading edge.[53] Note that value obtained from the
valence band XPS spectrum only represents the VB potential
relative to flat band potential (Efb), whereas careful analysis of
the UPS spectrum (as detailed to ref. [54]) allows determination
of the absolute value of the VB potential.
Current advancement in spectroscopy techniques has ena-
bled direct measurements of photoexcited charge carrier
dynamics using a wide range of time-resolved spectroscopic
techniques. Minor carrier diffusion length (LD), lifetime (τ),
rate constant for charge transfer (Ktr), rate constant for charge
recombination (Krec), and other carrier information can be
measured experimentally using time-resolved photolumines-
cence (TRPL), time-resolved microwave conductivity (TRMC),
transient absorption spectroscopy (TAS), photoinduced absorp-
tion spectroscopy (PIA), and intensity-modulated photocurrent
spectroscopy (IMPS). A comprehensive discussion on each
approach can be found in our recent review article.[53]
Although the abovementioned characterizations are inter-
changeably used for photocatalysts and photoelectrodes to
provide similar details, there remain certain situations where
different information should be obtained. For example, in a
photoelectrode with multilayer components, bulk analysis using
conventional XRD cannot differentiate the different layers.
Glancing angle XRD with an adjustable angle for the incident
X-ray is needed to quantitatively evaluate the layered com-
ponents. Similarly, Ar-etched XPS is useful in measuring the
composition of a photoelectrode with a distinctive multilayer
arrangement while this tool is not as useful for distinguishing
the elemental distribution within a powdered photocatalyst.
Microscopy combined with elemental mapping would be more
suitable for a powdered photocatalyst for this purpose.
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The evaluations of the number of redox products evolved are
the most straightforward approach for assessing photocatalytic
or photoelectrochemical systems. However, since the reaction
conditions such as reactor configuration, light intensity, and
light wavelength can be different, determining the quantum
efficiency of a photocatalyst or a photoelectrode is critical for a
valid comparison of materials examined under different condi-
tions. Apparent quantum yield (AQY), therefore, is adopted to
evaluate the efficiency of a photocatalyst, in which the AQY is
derived using the number of reacted electrons or holes divided
by the number of incident photons.[12] Note that AQY is esti-
mated to be smaller than the real quantum yield of a photocata-
lyst. This is due to the difficulty in quantifying the real number
of incident photons received by a photocatalyst in a suspension
solution, where light scattering phenomenon exists (i.e., the
number of photons absorbed is less than the number of inci-
dent photons). In contrast, the efficiency of a photoelectrode
is widely reported in the form of incident photon current effi-
ciency (IPCE) as a function of wavelength. IPCE is derived
from the photocurrent density and the intensity of monochro-
mated irradiation at a particular wavelength.[2] In addition to
IPCE, absorbed photon-to-current conversion efficiency (APCE)
and applied bias photon-to-current conversion efficiency
(ABPE) have also been developed to evaluate the solar conver-
sion efficiencies of a photoelectrode.[55,184] However, they are yet
to be adopted in the evaluation of photocatalytic systems. It is
challenging especially when a photoelectrode is made of immo-
bilized powdered semiconductors on a conducting substrate,
the efficiency measurement based on photocurrent generation
can be greatly affected by the quality of the interfacial contact
between the two components.
2.5. Reactor Designs for Photocatalytic and
Photoelectrochemical Systems
In both photocatalytic and photoelectrochemical systems, the
photoactive semiconductor is the central component requiring
excitation by incident light to produce photogenerated electron–
hole pairs. Upon fulfilling certain requirements, these excited
charges can be transferred to reactants (in this review, aqueous
phase reactants are emphasized) via oxidation (hole transfer)
or reduction (electron transfer). For example, water molecules
will be split into oxygen and hydrogen, CO2 converted into CO,
CH4 or longer chain carbon species, N2 reduced into ammonia
or hydrazine, and organic waste oxidized into other desired
organic products by photoactive semiconductors. In the photo­
electrochemical system, an externally applied voltage can be
provided to assist the redox reactions, in which the externally
applied voltage is an additional energy input to the system. In
a photocatalytic process, solar energy is the lone energy input
source. The photocatalytic process appears to be much sim-
pler without the need to incorporate additional electrochemical
energy. However, it also has a stricter thermodynamic require-
ment to drive the chemical reactions without an external aide.
In a typical photocatalytic system, powdered photocatalyst is
suspended homogeneously in an aqueous solution containing
reactants (for water splitting, water is the reactant, while for
CO2 reduction and N2 fixation, aqueous solution saturated
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with CO2 and N2 are the respective reactants) under agitated
conditions. The suspension (or slurry, depending on the photo­
catalyst concentration) should be capable of absorbing suffi-
cient photons from an artificial light source or natural sunlight
to facilitate the redox reactions with minimal charge losses.
There are several reactor designs typically used by researchers
on a laboratory scale (Figure 12a).[12] A closed-gas circulation
system with a Pyrex reactor cell, as shown in Figure 12b, is
the essential apparatus in a photocatalytic system.[185] Gas or
liquid chromatography or a volumetric method can be used to
quantify the evolved liquid and gaseous products. Most photo­
catalytic reactors are designed with a top-down illumination
configuration where a Xe-lamp (with cut-off filter to select illu-
minated spectrum), solar simulator (with air-mass 1.5 filter)
or actual sunlight can be directed to the powder-suspension.
For photocatalytic wastewater treatment where closed-gas
circulation system is not required, a simpler setup that enables
homogenous mixing and liquid sampling throughout the reac-
tion (e.g., round bottom flask) is commonly employed. In addi-
tion, flow systems such as suspension spiral reactor that allows
more light exposure, fixed-bed and fluidized-bed and hybrid
photocatalytic-membrane reactor have also been used for water
disinfection.[187,188]
Recently, from a practical point of view for large scale water
splitting, Domen and co-workers designed and demonstrated
the first photocatalytic water splitting panel/module with the
dimension of 1 m × 1 m consisting of SrTiO3:Al photocatalyst
sheets and an outer frame (Figure 12c).[186] In their design,
unlike the typical Pyrex cell used in a laboratory, the powder
photocatalyst was not suspended in water but immobilized on
a glass substrate for easier handling. The depth of the water
layer is as thin as 1–5 mm to reduce water pressure induced
by the weight of the water. The photocatalytic water splitting
panel was tilted at 10°–20° so that the generated gases could
be released without trapping. As a safety measure, the hydro-
philicity of the top window was controlled in order to prevent
the retention or accumulation of bubbles. The current solar-to-
hydrogen (STH) efficiency of the field test (performed under
natural sunlight at 1 m2 scale) was ≈0.4%. The work represents
an important milestone in solar hydrogen using a photocatalyst
(as compared with a PV-electrolyzer and PEC cells) and dem-
onstrates the viability of the large-scale production of low-cost
solar hydrogen using water splitting technology. Apart from
large scale photocatalytic water splitting technology, indus-
trial scale solar water disinfection plant has been developed a
few decades ago.[189,190] The nonconcentrating solar photodis-
infection system has then been evolved into parabolic trough
concentrating system and eventually compound parabolic con-
centrators (CPCs) tubular systems, as illustrated in Figure 13a.
The CPCs system enable concentrated sunlight to be reflected
around the tubular absorber/reactor for optimized disinfection
performance, in which operational CPCs pilot plant has already
been installed in 2004 at Almeria, Spain (Figure 13b).[191,192]
In a photoelectrochemical system, reactors with various con-
figurations have been designed to allow for maximum photon
absorption per unit volume of the reactor. Unlike photocatalytic
reactions where the redox reactions occur in the same reaction
chamber, one of the unique features of a photoelectrochemical
reactor is the products are readily separable. This is because the
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Figure 12. a,b) Examples of an experimental setup in the laboratory for powder-suspension type photocatalytic water splitting, c) 1 × 1 m photocatalytic
water splitting panel with immobilized photocatalyst. a) Reproduced with permission.[12] Copyright 2009, Royal Society of Chemistry. b) Reproduced
with permission.[185] Copyright 2013, Elsevier B.V. c) Reproduced with permission.[186] Copyright 2018, Cell Press.

oxidation and reduction reactions occur at the photoanode and
photocathode, respectively. The anodic and cathodic chambers
are separated by a membrane where back reactions could be
avoided. Spaces or distances between the photoanode and
photo­ cathode should also be minimized to decrease the
potential loss or ionic resistance during photoelectrochemical
reactions. Selected excellent reviews on photoelectrochemical
reactors are available and this section will briefly detail the dif-
ferent configurations reported to date.[193–196]
Figure 14 summarizes the design of photoelectrochemical
reactors using a single photoelectrode, dual photoelectrodes,
and the configurations of the photoelectrodes in receiving
incident light.[196] In a single photoelectrode reactor, either the
photoanode or the photocathode is illuminated (Figure 14a).
Upon photoexcitation, electrons generated on the photoanode
will be transferred from the semiconductor to the conducting
substrate underneath and subsequently driven by the external
voltage to the counter electrode to induce the reduction reaction
(e.g., H+ reduction to form H2, and N2 reduction to ammonia
or hydrazine). Photogenerated holes are pushed toward the sur-
face of the photoanode for the oxidation reaction. An opposite
flow of electrons applies when a single photocathode reactor
is used. This kind of single photoelectrode system is usually
employed to study the effectiveness of the designed photo-
electrode (either anode or cathode) and is not meant for the
actual application. It has some major disadvantages that pre-
vent it being used at a larger scale: 1) the necessity to apply
an external bias to withdraw the charges; and 2) the use of an
expensive counter electrode (platinum is commonly used). A
solution or argument can be made for 1) in that the external
voltage can be supplied by an electrical bias, chemical bias or
PV bias. In those circumstances, the development of an elec-
trolyzer appears to be more straightforward as the electrolyzer
does not involve fabricating a semiconductor immobilized on
a conducting substrate as well as eliminates the need to direct
photons in the reactor design.
Figure 14b shows the various configurations possible for a
dual-photoelectrode system. The dual-photoelectrode system

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Figure 13. a) Schematic design of nonconcentrating, concentrating (parabolic trough), and compound parabolic concentrating systems. b) Schematic
drawing and photograph of a compound parabolic concentrator. a) Reproduced with permission.[191] Copyright 2009, Elsevier B.V. b) Reproduced with
permission.[192] Copyright 2007, Elsevier B.V.

with a suitable reactor configuration may be more suited to
larger-scale usage.[196] In a dual-photoelectrode system, both
the photoanode and photocathode are assembled so as to be
photoexcited. With the proper selection of an n-type photo-
anode and a p-type photocathode, in which the CB position of
the photoanode is greater than the VB position of the photo­
cathode, the internal voltage generated is sufficient to drive
electrons through the external circuit for the redox reactions to
occur at their respective electrodes.[197] This offers the option
of a bias-free photoelectrochemical system for meaningful reac-
tions such as water splitting. As can be seen in Figure 14b,
the photoanode and photocathode can be placed in parallel or
in series. In the parallel setting, inexpensive nontransparent
conducting substrates can be used as the incident light does
not need to transmit through the photoelectrodes. However, a
larger area exposed to the incident light is needed to accom-
modate both photoelectrodes and may not be easy for reactor
miniaturization. In the series setting, the photoanode and
photo­cathode are placed in a tandem arrangement. The incident
light should pass through the wide bandgap photoelectrode
first. The less energetic photons with the longer wavelengths
can pass through the first photoelectrode to reach the second
narrow bandgap photoelectrode. With this tandem structure,
the photoanode and photocathode should be connected either
through a conductive metal wire (wired) or both photoelec-
trodes are loaded on a single transparent conductive substrate
(wireless) system. The tandem configuration is advantageous
as each photoelectrode provides a photovoltage to achieve an
external bias-free photoreactor.
3. Limitations, Potential Solutions, and Future
Outlook
The library of photoactive semiconductors has become plentiful
over the last few decades credited to the advances in materials
chemistry for both materials synthesis and characterization. The
expansion of the photoactive semiconductor database continues
to inform the community on factors affecting photoactivities
(be it in the configurations of suspension-type photocatalytic or
photoelectrochemical systems). Collectively, the understanding
of photoinduced activities is established. However, the targeted
solar energy efficiency of about 5% using photocatalysis or
photoelectrocatalysis remains far from being achieved. There
are still a number of concerns in the photocatalytic and photo-
electrochemical systems that need to be addressed.

Adv. Mater. 2019, 1904717 1904717 (15 of 21) © 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.advancedsciencenews.com
Figure 14. a,b) Configuration of photoelectrochemical reactors with a single photoelectrode (a) and a dual-photoelectrode (b). a,b) Reproduced with
permission.[196] Copyright 2019, Elsevier B.V.
Many efficient photoactive semiconductors in the sus-
pension-type system currently tend to contain various noble
metals such as Ta, Rh, and Ru.[117,198–201] In particular,
NaTaO3 doped with La exhibits the most active photocata-
lytic water splitting performance with NiO as cocatalyst.[94]
However, eliminating the use of such expensive elements
by replacing them with abundant elements such as Co, Fe,
and Cu is imperative to realize the goal of commercializing
photo­ catalysts for the solar energy conversion industry.
Another challenge is the limited light absorption efficiency
at the range of 600–700 nm for the most developed single
photocatalyst. Discovering new photoactive semiconductors
particularly active under red and near-infrared irradiations is
therefore important to achieve higher solar energy conversion
efficiency. Compared to the single photocatalyst, Z-scheme
photocatalyst and other heterojunction composite photocata-
lysts are advantageous as a wider range of light spectrum can
be utilized. For instance, under visible illumination, ternary
oxides such as BiVO4 is applied as an efficient oxygen photo-
catalyst in Z-scheme water splitting when it is coupled with
doped SrTiO3 as a hydrogen photocatalyst.[117,200] Nonetheless,
the suppression of backward reactions and matching the per-
formance for overall photocatalytic reactions is critical. The
construction of redox mediator free Z-scheme systems and
Adv. Mater. 2019, 1904717 1904717 (16 of 21)
www.advmat.de
the fine adjustment of reaction conditions are considered as
feasible solutions.
Among various n-type metal oxide semiconductors, BiVO4
with a narrow bandgap is regarded as a potential photoanode
material.[202] However, its catalytic function and charge move-
ment properties are yet to be ideal as an efficient photoanode.
Strategies including cocatalyst deposition, doping, thermal
treatment, and homo/heterojunction are highly recommended
to be employed on the pristine BiVO4 to improve its photo-
electrochemical activity. Besides, semistable Ta3N5 recorded an
anodic photocurrent density of ≈12 mA at 1.23 VRHE,[203] which
presents a higher performance than all other reported metal
oxide materials. However, in the future development of effi-
cient metal nitride photoanode materials, rare metals such as
Ta should ideally be replaced by other abundant elements such
as the fourth-period metals. As the photocathode, Cu2O (with
protecting layers) achieved the highest cathodic photocurrent
density of 10 mA cm−2 at 0 V RHE.[197] Nonetheless, the atomic
layer deposited protecting layers are indispensable to its good
performance, which inevitably increase the cost and complexity
of fabricating such photocathode materials. Therefore, the devel-
opment of facile but versatile coating techniques which is alter-
native to atomic layer deposition is meaningful for the future
scale-up attempts. The theoretical prediction or theory-guided
© 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.advancedsciencenews.com
design of new materials is crucial for the community to design
new materials or to improve existing materials suitable for solar
energy conversion. However, most computational calculations
(e.g., DFT) remain limited to ground state simulation. Though
the information is highly applicable, modeling under excited
states could provide more accurate information in designing
new functional photoactive materials.
Not limited to this field of research, the in situ or oper-
ando characterization of materials during the photoreac-
tions is highly important to allow researchers to understand
the dynamic changes to material properties under reaction
conditions. The offline characterization is affected by many
uncertainties as well as does not represent the exact reac-
tion conditions. A number of excellent characterization tools,
including advanced electron microscopies and time-resolved
spectroscopies, can provide insightful data on the optical/
electronic properties of a semiconductor. The absence of a
solid–liquid interface in the measurement may also need more
thought from the community so as to understand the exact
mechanistic information.
The challenges in reactor design also limit the progress of
translating laboratory testing to pilot and industrial scales.
The large volume of aqueous solution in the form of a photo­
catalyst suspension is difficult to handle at large scale. Semi-
conductor particles which settle at the reactor base are not
effective in harvesting light. The practicability of maintaining
an agitation over large area is also problematic. Retrieving the
spent powder using existing methods is also energy and time
consuming. Therefore, the careful and smart design of a prac-
tical photoreactor is indispensable even with the discovery of
a highly efficient semiconducting material. In fact, a panel
reactor conceptually named as Schröder’s reactor,[204] consisting
of photocatalyst sheets and an outer frame, is recommended
for large-scale solar water splitting. The photocatalyst sheets
covered with only a 1–5 mm thick layer of water can produce
gas bubbles, which avoid the handling of a large volume of
aqueous solution in the traditional reactor. Also, the photocata-
lyst panel is generally tilted at 10°–20° to guarantee the rapid
release of evolved products and an effective harvesting angle of
sunlight. Obviously, the retrieve of the particulate thin film is
not a problem for the panel reactor. Despite the multiple advan-
tages, it is still necessary to integrate a safe and adequate gas
separator in a photocatalytic system to realize a whole solar-to-
chemical conversion process.
The reactor design of photoelectrochemical systems has
been divided into two categories. The first type of the reactor is
designed for measuring the fundamental parameters of either
photoanode or photocathode in a three-electrode configuration,
in which an external voltage is supplied to assist the charge
separation and migration; the second type of photoelectro-
chemical reactors is closer to the prototypes of dual-electrode
devices (photoanode–photocathode tandem cell) for unassisted
photoelectrochemical reactions. It is constructed for accom-
plishing solar energy conversion efficiencies. For a tandem cell,
a photocathode and a photoanode are integrated into a device
by a conductive wire (e.g., Cu wire) or wireless attachment with
good ohmic contact. Grätzel and co-workers recently reported
a “wired” tandem cell composed of a NiMo/TiO2/Ga2O3/Cu2O
photocathode and NiFeOx/H,Mo:BiVO4 photoanode, which
Adv. Mater. 2019, 1904717 1904717 (17 of 21)
www.advmat.de
exhibited an STH efficiency of 3%.[197] This work essentially
demonstrates the advantage of a tandem photoelectrochem-
ical cell in achieving good solar energy conversion efficiency.
However, those reported photoelectrochemical tandem systems
are yet to meet the target STH efficiency of 10%. Reducing
internal resistance loses of the designed reactor and optimizing
the light-harvesting of photoanode and photocathode are the
possible approaches. Beside the water splitting process, the
photoelectrochemical N2 reduction, CO2 conversion and pol-
lutant degradation are also very attractive, in which the Nafion
membrane is normally adopted to separate the redox products.
Nevertheless, the possible physical and chemical interactions
between the Nafion membrane and the redox products should
be carefully avoided when designing the photoelectrochem-
ical reactors. Very recently, Ren et al. reported that the Nafion
membrane allows ammonia to pass through and absorbs the
ammonia to some extent, which may cause a measurement
error up to around 30%.[205] Similar considerations should be
taken into the design of photoelectrochemical reactors for CO2
conversion and pollutant degradation processes in the future.
Photocatalytic and photoelectrochemical systems used for
solar-to-chemical energy conversion applications are devel-
oped in parallel. While both systems employ photoactive
semiconductors as the core component in their functionality,
some common strategies have been formulated and adopted
to improve their performance. This review correlates aspects
including particle size, crystallinity, dimension (0D, 1D, 2D,
and 3DOM), crystal facet, multicomponent junction, characteri-
zation, evaluation, and reactor design with the essential physi­
cochemical processes (light absorption, charge separation and
migration, surface passivation and protection, and redox reac-
tions etc.) when using the same photoactive semiconductor in
different configurations. In this circumstance, different sets of
requirements or standards to achieve promising performances
need to be contemplated. Consequently, some of the material
improvement strategies generally adopted within the research
community may result in similar trends in experimental out-
comes although deliver different degrees of effectiveness when
employed in photocatalytic and photoelectrochemical systems.
Other strategies may result in opposite trends and be con-
structive in one system but detrimental to the other system.
For instance, 0D particles with a larger specific area have been
widely used for suspension-type photocatalytic systems while
the losses of energetic charge carriers among countless inter-
particle interfaces have limited the performance of 0D particles
assembled into photoelectrodes.
Note that despite the different or even opposite effectiveness
of factors governing the performance of photoactive semicon-
ductor in photocatalytic and photoelectrochemical systems, they
are reconcilable by employing proper strategies with an under-
standing of the underlying reasons. As an example, nanostruc-
tured photocatalysts (such as 3DOM materials) endowed with
enlarged surface area, increased light scattering and facilitated
intrinsic charge extraction have demonstrated great potential
in photocatalytic systems especially for pollutant degradation
reactions. Nevertheless, the limited contact between the pointy
edges of nanostructured photocatalysts and the conducting
substrate will compromise the beneficial effects in a photoelec-
trochemical system. With this understanding, the strategy of
© 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.advancedsciencenews.com
direct synthesis of such nanostructured photoactive semicon-
ductors on the conducting substrate is recommended to estab-
lish an intimate contacted interface between the immobilized
photocatalysts and the conducting substrate. More specifically,
taking 3DOM photocatalyst as an example, some deposition
techniques including (pulsed)-electrodeposition, physical layer
deposition and atomic layer deposition can therefore be taken
into consideration to deposit the photoactive materials on
a spherical polymer (e.g., PMMA or polystyrene) templated
substrate followed by a thermal or acid treatment to remove
the organic template. This review is intended to provide useful
information for guiding the design of efficient photocatalytic
and photoelectrochemical systems.
Supporting Information
Supporting Information is available from the Wiley Online Library or
from the author.
Acknowledgements
H.W. and H.L.T. contributed equally to this work. The authors thank the
Australian Research Council for financial support through Discovery
Projects DP180102540 and DP170102895.
Conflict of Interest
The authors declare no conflict of interest.
Keywords
mechanism similarity, photoactive materials, photocatalysts,
photoelectrochemical systems, solar energy conversion, system
performance, water splitting
Received: July 23, 2019
Revised: September 17, 2019
Published online:
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