Tech Science Press

DOI: 10.32604/jrm.2022.018556

REVIEW

g-C3N4 Derived Materials for Photocatalytic Hydrogen Production: A Mini

Review on Design Strategies

Kai Su1,*, Shaoqi Deng1, Linxiao Li1, Qirui Qin1, Jingyu Yang1, Yan Chen2,3, Shengli Zhang1 and
Junming Chen1
1
Faculty of Geosciences and Environmental Engineering, Southwest Jiaotong University, Chengdu, 611756, China
2
Analysis and Testing Center, South China Normal University, Guangzhou, 510006, China
3
MOE Key Laboratory of Theoretical Chemistry of the Environment, School of Chemistry, South China Normal University,
Guangzhou, 510006, China
*
Corresponding Author: Kai Su. Email: [email protected]
Received: 02 August 2021 Accepted: 20 August 2021

ABSTRACT
Hydrogen production through solar energy is one of the most important pathways to meet the growing demand
of renewable energy, and photocatalyst participation in solar hydrolytic hydrogen production has received great
attention in recent years in terms of low cost, high efficiency, and flexible design. Particularly, g-C3N4 (Graphitic-
like carbon nitride material), as a unique material, can catalyze the hydrogen production process by completing
the separation and transmission of charge. The easily adjustable pore structure/surface area, dimension, band-gap
modulation and defect have shown great potential for hydrogen production from water cracking. In this review,
the most recent advance of g-C3N4 including the doping of metal and non-metal elements, and the formation of
semiconductor heterojunction is highlighted. The main modification strategies and approaches for the design of
g-C3N4 for hydrogen production, as well as the influence of various materials on hydrogen evolution regarding
the photocatalysis mechanism and advantages brought by theoretical calculations are specially and briefly illu-
strated. Potential design pathways and strategies of g-C3N4 are discussed. In addition, current challenges of
hydrogen production from g-C3N4 water splitting are summarized and can be expected.

KEYWORDS
g-C3N4; hydrogen; photocatalysis; H2O; semiconductor

1 Introduction
The rapid economic growth has encouraged researchers to find new forms of energy, along with the
global goals for low/zero carbon dioxide emissions. The adoption of renewable energy is one of the most
important pathways [1]. As renewable energy, hydrogen energy has high calorific value and clean
properties [2]. Massive studies have adopted photocatalytic process to decompose pure water or waste
water to relieve environmental pollutants and to obtain hydrogen energy, simultaneously [3,4]. Among
the numerous materials, inorganic semiconductor materials are of low cost compared with rare metal
catalysts [5]. The g-C3N4 polymer can induce visible light and its unique electronic structure and adaptive

This work is licensed under a Creative Commons Attribution 4.0 International License, which
permits unrestricted use, distribution, and reproduction in any medium, provided the original
work is properly cited.
654 JRM, 2022, vol.10, no.3

capacity to adjust the band structure has attracted wide interest [6,7]. Moreover, the easy acquaintance from
nature, no toxicity and strong stability of the C and N elements make them stand out.
In this regard, some preparation methods for g-C3N4, including the thermal condensation, solvothermal
synthesis, microwave assisted synthesis, ionic liquids, and molten salt methods have been widely reported
[8–10]. Meanwhile, the utilization of the precursor such as urea, melamine, thiourea and the preparation
with other materials are crucial [11,12]. At present, the structure of the g-C3N4 models has been widely
recognized, as shown in Fig. 1. Abundant modification pathways are taken to reduce the g-C3N4
interchange material used in catalytic hydrogen production defects, including metal or nonmetal doping,
while the micro structure is modified to address the issues of generally low specific surface area, the raw
carrier transfer, light electronic-hole, forbidden band width and other problems. In this review, relevant
modifications of g-C3N4 were summarized, and the enhancement mechanisms in a hydrogen production
scenario and future application challenges of the design strategies g-C3N4 materials were presented.

Figure 1: Structural model of g-C3N4: (a) S-triazine ring structure (blue shadow unit); (b) 3-s-triazine ring
structure (red shadow unit)

2 Mechanism of g-C3N4 Photocatalysis for Hydrogen Production

As one of the most important application scenarios of g-C3N4 photocatalysis, hydrogen production has
received a lot of attention. Based on the Gibbs free energy change (H2O → H2 + 1/2O2, ΔG = 238 kj/mol) and
thermodynamics, the splitting should meet the energy source [12]. Therefore, extra photon energy is needed
to break an energy barrier of 1.23 eV. Thus, the band-energy gap of the g-C3N4 or the derivatives should be in
the range of 1.23–3.0 eV to maintain effective splitting of water [13]. Valence band (VB) and empty
conduction band (CB) can be separated by forming finite band energy gap [14]. When irradiation of
incidence light is developed during the generation of photo-excited charge carrier, the exciting electrons
from VB to CB can separate the e− and h+ pair involved in reduction and oxidation [15]. In this regard,
the photocatalytic process generally includes several processes [16] (Fig. 2): (a) photon absorption; (b)
exciton separation; (c) carrier diffusion, in which the low charge recombination rate decreases the charge
separation rate and leads to a poor transmittance; (d) carrier transport; (e) catalysis efficiency, which
decides the apparent quantum efficiency; (f) the light-generated e−/h+ pairs are adsorbed, followed by the
movement of e− to CB with the holes in VB, which enhances the h+ and e−. Through these steps,
appropriate modification strategy to enhance the overall water splitting efficiency can be predicted.
There have been extensive studies on the mechanism of photocatalysis. g-C3N4 is very active under
visible light due to the wide band gap. Considering the wide band gap of g-C3N4 and over-potentials, the
band-energy gap ranges from 2.0 eV to 3.1 eV is higher than that of the endothermic driving forces
which is about 1.23 eV but lower than visible light absorption scope [17]. The CB is higher than the
potentials of H2 production in the negative position. It is known that the sp2 hybridization in 2D can form
layered construction due to the poor van-der Waal’s forces between C and N in g-C3N4, and the thermal
JRM, 2022, vol.10, no.3 655

conversion process can help the condensation of feedstock with a molar ratio of 0.75 [18]. The photo-
generated holes of g-C3N4 facilitate oxygen generation from H2O oxidation and avert the CO2
mineralization by strong •OH. But the low efficiency aroused by high e−/h+ recombination rate of smooth
g-C3N4 has been noticed and a lot of downstream technologies focus on the enhancement of active sites,
grain boundary defects and kinematics [16,17]. Additionally, researchers have widely followed the first
principle based on density functional theory in the field of photocatalysis as a clear research method for
effective and quick exploration to improve the g-C3N4 photocatalytic performance [19,20]. With the
incomparable advantage of semi-empirical method like Grimme, first principle based on density
functional theory has become an important basis for calculation and simulation [21]. Thus, the lattice
constant, density, cell volume, relative energy, electron structure, and absorption spectra based on g-C3N4
can be obtained. With the calculation of band structure, density of states, and etc., it will provide more
theoretical guidance for the properties and modification of g-C3N4. As described above, typical normal
potentials of redox reaction with g-C3N4 band-energy gap under pH of 7 are presented in Fig. 3 [22].

Figure 2: Mechanism of photocatalytic reaction for g-C3N4

Figure 3: Typical band structures of various type of semiconductor photocatalysts compared with g-C3N4

3 Modification Pathways for g-C3N4

To modify the energy band structure of g-C3N4, doping metallic or nonmetallic elements by physical or
chemical pathways has been proved to be effective. The light absorption, charge density, charge dispersion
and mobility, as well as the crystallinity can be changed by introducing external doping elements into the
semiconductor lattice. Generally speaking, nonmetals doping is realized by embedding in the body
656 JRM, 2022, vol.10, no.3

structure of g-C3N4, including B, O, S, P, Cl, Br, I, and F [23–25]. It is critical to determine the location and
defects of the introduced element in the skeleton structure of g-C3N4. For example, P element can exist in the
structure matrix of g-C3N4 in the form of P-N bond, which makes the band gap narrow and promotes exciton
separation, and some studies have found that P doping delayed the rapid recombination of electron hole pairs
[25]. As for B and N, the introduction defects can broaden the visible light absorption range of g-C3N4, and
abundant unsaturated sites can enhance the interaction of the interlayer C-N, and further promote the
separation of excitons and charge transmission [26].
Generally, Mn, Zn, Cu, Ni, Fe, Co etc. are the main metal doping elements in present works [27]. Since
g-C3N4 is a hepazine ring composed of three triazine rings along with a cavity structure formed by six
unsaturated N-coordination structures, it is easy to facilitate metal elements to form metal coordination
electronic structure. For example, Mn can be embedded in g-C3N4 as Mn-N-C group, which can adjust
the positron and energy band structure, and further promote the charge transfer [27]. On this basis,
researchers also try to study the influence of metal doping on g-C3N4 in order to optimize the strength of
the metal-C-N bond or to adjust the spin state of metal ions. However, the amount of element doping is
also a crucial factor. For instance, Fe doped g-C3N4 nanosheet structure will be cracked beyond certain
Fe mass ratio. Until now, various characterization techniques including nuclear magnetic resonance, XPS,
FTIR, NMR, XANES, etc., have showed that the doping elements were not only related to the size of the
atomic radius of the element, but also related to the pathways and forms of the embedding. The typical
doping sites of nonmatals and metals in g-C3N4 are shown in Figs. 4 and 5. In addition to element
doping, modification of the morphology of g-C3N4 is another strategy, which can also modify the
electronic structure, optical properties, and desirable surface characteristics. Different dimensions of
g-C3N4 structures like carbon dots, nanorods/wires/bands/tubes/sheets/spheres/gels, etc., are defined as
0D-3D materials and show obvious differences in preparation conditions, specific surface area, exposure
degree of active site, and lifetime of photogenerated carriers [28,29]. With this, secondary modification of
materials with different dimensions of g-C3N4 and doping elements will have great potential.
Nevertheless, the preparation of materials cannot be perfect due to the absence of N, C and cyanogroup,
which is also called defect engineering, but this will provide opportunities for the improvement of optical
properties of g-C3N4 [30,31].
Additionally, after the light excitation process, the electron-hole pair has a high repetition rate, which can
affect the photocatalytic performance of the material. Numerous studies have proved that the formation of
heterojunction structure with composite of semiconductor materials such as TiO2, ZnO, NiS, Ni2P, etc.,
and even metal organic framework (MOF) was an effective strategy to improve the photocatalytic
performance of bulk g-C3N4 [32,33]. The heterojunction structure can be formed by seamless
combination of g-C3N4 with carbon materials through π conjugated bonds [33]. Through the formation of
heterojunction, the surface or cross linked to the crystal lattice interface inside the semiconductor can be
tightly bonded and can induce the formation of internal electric field. The typical heterojunction of Type
II and Z-scheme charge transfer for g-C3N4 are shown in Fig. 6 [34]. Specifically, the electrons in the
excited state can be firstly transferred to the conduction band under the light condition, and the
semiconductor with more negative conduction band position then moves forward as more positive
semiconductor, while the photogenerated hole is on the opposite and accelerates the effective separation
of the photogenerated electron hole pair, which is very favorable in the field of photocatalytic hydrogen
production [35,36]. In a nutshell, the purpose of modification of g-C3N4 materials is to enhance the
utilization of light and to increase the active sites and reduce the recombination of photogenerated
electron-hole pairs, which will be the basis for further breakthroughs in g-C3N4 material innovation in the
future.
JRM, 2022, vol.10, no.3 657

Figure 4: Potentials substituted sites of non-metals doping in a single g-C3N4 layer

Figure 5: Typical diagram of metal ion (Ma+) incorporation in g-C3N4 framework

Figure 6: Typical heterojunction of Type II and Z-scheme charge transfer for g-C3N4
658 JRM, 2022, vol.10, no.3

4 Design Strategies of g-C3N4 for H2 Generation

The significant progress of g-C3N4 nanostructures tailoring techniques for catalytic H2 generation has
got a great deal of attention during the past ten years. In this section, the myriads of applications for H2
production via water splitting were reviewed with various design strategies of g-C3N4 materials. For solo
inorganic element doped g-C3N4, the H2 generation rate can be increased by 10–20 times and more. For
instance, the H2 generation rate derived from sulfur-doped polymeric g-C3N4 photocatalysts reached
12.16 μmol h−1 [36], while the value was 57 μmol h−1 for P-doped g-C3N4 tubes [37], and 70.05 μmol h−1
for B doped g-C3N4 quantum dots [26], respectively. A lot of studies have also proved that g-C3N4
simultaneously doped with various species of inorganic elements or metals could also ameliorate visible-
light photocatalytic H2 generation [38,39]. For example, in Yang et al. [24]’s study, a higher surface area
with optimized sp2 conjugated heterocyclic structure was obtained for g-C3N4 prepared with C-I, and the
hydrogen evolution rate reached 168.2 μmol/h. Generally, researchers prepared catalyst by using porous
g-C3N4 to further modify and obtain higher efficiency of hydrogen production. Wu et al. [40] fabricated
porous g-C3N4 nanobelts by using method of C, O binary-doped hierarchical, and the replacement of N
atoms narrowed the bandgap and favored the harvest of visible-light for high H2 evolution. In Deng et al.
[41]’s work, the low electron-hole recombination rate and rapid electron transfer were found to account
for the high hydrogen evolution reaction of Ni/porous g-C3N4. Unlike that, several works found that
heterostructure could be fabricated by formation of crystal. For example, Jia et al. [42] found that FeSe2/
g-C3N4 formed nanosheets and accelerated the decomposition of H2O2 generation on the nanosheet
surface via a stepwise two-electron/two-step pathway. In conclusion, a number of enhanced hydrogen
production pathways have been demonstrated by developing and designing a robust photocatalyst.
Representative g-C3N4 material preparation and the superiority for H2 generation rate are summarized in
Tab. 1. Meanwhile, based on the section discussed above, the design strategies of g-C3N4 for H2
generation are summarized in Fig. 7.

Table 1: Representative g-C3N4 materials preparation and the superiority for H2 generation rate
Precursors Synthesis H2 generation rate Superiority References
methodologies
Urea; molybdenum Pyrolysis 327.5 μmol⋅g−1⋅h−1 Increased light absorption, separation and transfer of [43]
photogenerated carriers
Urea; Ni(NO3)2 and 550°C for 4 h 992 μmol g−1 h−1 Improved visible light absorption, promoted charge [44]
Na2S separation
urea and NH4Cl 550°C for 3 h - Extend the π-conjugation; reduce the band gap and [45]
facilitate the separation of photogenerated charges
Dicyandiamide; 600°C for 3628 μmol g–1 h–1 Chemical bonding of Ni-S favored charge-separation [46]
Nickel ammonium 270 min
sulfate, H2S
Melamine; silver 650°C for 3 h 9.728 Co-decoration of Ag and NiS; improved light [47]
nitrate mmol⋅g−1⋅h−1 harvesting capacity, photogenerated charge carrier
separation
Melamine; Ni-MOF 550°C for 2 h 14.49 mmol g−1 Increased the electron transfer rate staggered band [48]
h−1 alignment
Urea; graphdiyne 550°C for 2 h 39.6 μmol h−1 Prolonged photogenerated charge carrier lifetime, [49]
intensified electron density, decreased reaction
overpotential and improved charge carrier mobility
Melamine; 550°C for 4 h 941.80 μmol g-1 h-1 Enhanced light absorption and high-efficiency transfer [50]
and separation of photogenerated electron hole pairs
(Continued)
JRM, 2022, vol.10, no.3 659

Table 1 (continued)

Precursors Synthesis H2 generation rate Superiority References

methodologies
Melamine; TiO2 300°C–700°C 52.71 μmol h−1 Wide optical absorption, separation and transportation [51]
for 2 h of electronic-holes, and morphology of composite
Melamine; N-ZnO 550°C for 5 h 152.7 μmol h−1 Promoted the spatial charge separation [52]
Urea; CoS2 550°C for 4 h 11.55 μmol h−1 Improved the visible-light absorption ability and [53]
generation of photo-generated carriers
Melamine; Co 520°C for 2 h 11291 μmol h−1 g−1 Improved interfacial charge transfer rate with low [54]
doped Mo-Mo2C photo-generated charge recombination

Figure 7: Design pathways and strategies of g-C3N4 for H2 generation

5 Conclusion and Future Challenges

In this review, the modification pathways of g-C3N4 related to the elemental doping, heterojunction
development and other methods were elaborated. The enhancement mechanisms in a hydrogen
production scenario and future application challenges of the design strategies g-C3N4 materials are
presented. Despite that the g-C3N4 materials used for photocatalytic hydrogen production have been
investigated by numerous scientific works for water splitting application, the preparation, optimization of
660 JRM, 2022, vol.10, no.3

raw materials, and the cost of hydrogen production, as well as related mechanisms of research require further
extensive exploration. The detailed future challenges to overcome are as below:
(1) The durability and stability of g-C3N4 should be taken into more consideration regarding the
recycling and efficiency.
(2) The choice of precursor feedstock for g-C3N4 is critical. It is essential to understand the thermal
method and all other methods that can provide a better strategy for the g-C3N4 preparation.
(3) More morphological research should be conducted on the new heterojunction and homojunction with
surface or interface characteristics and narrow absorption range.
(4) Carbonaceous semiconductors should be investigated on the metal and non-metal doping, defects,
and interaction mechanisms of multiple functions, and can provide references of optimized
hydrogen production rate and lower catalyst cost in the future.

Funding Statement: This work was supported by Sichuan Science and Technology Program
(2021YFS0284, 2018SZDZX0026, 2021YFS0289), the Opening Project of Key Laboratory of
Theoretical Chemistry of Environment (South China Normal University), Ministry of Education
(20200103), the Fundamental Research Funds for the Central Universities of Southwest Jiaotong
University (210824), and the Opening Project of Key Laboratory of Southwest Jiaotong University
(ZD2021210001).
Conflicts of Interest: The authors declare that they have no conflicts of interest to report regarding the
present study.

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