Adv Funct Materials - 2023 - Anne

REVIEW
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A Review on MXene as Promising Support Materials for

Oxygen Evolution Reaction Catalysts
Bhargavi Rani Anne, Joyjit Kundu, Mrinal Kanti Kabiraz, Jeonghyeon Kim, Daeheum Cho,
and Sang-Il Choi*
Therefore, developing catalyst supports

The harsh operating conditions of the oxygen evolution reaction (OER) in that strongly immobilize the catalyst par-
water electrolysis severely degrade the activity and stability of the ticles has been considered essential to
electrocatalysts due to elemental leaching or particle agglomeration. effectively improve the activity and sta-
Therefore, it is crucial to incorporate support materials that effectively bility of the catalysts and to solve particle
agglomeration.[23–26] Another important
immobilize catalyst particles for developing efficient OER catalysts. This
role of the catalyst support is that it can
review aims to highlight the role of MXene as a support material to improve achieve improved charge transfer kinetics
the performance of OER catalysts. First, the extended OER mechanism is through strong metal-support interaction
briefly described in terms of the effect of MXene support on OER catalysts. (SMSI), which can further enhance OER
Then, various synthesis methods of MXene and catalyst-MXene compounds activity.[27–31] For these reasons, conductive
supports such as Ni foam (NF), carbon nan-
are introduced, and important properties of MXene that are beneficial to
otube, graphene, graphdiyne, and MoS2
improve OER performances are discussed. The electrocatalytic results of the have inevitably been applied so far, despite
enhanced OER catalysts due to the effective MXene support are also the disadvantage of being corroded under
summarized. Finally, future challenges and prospects are proposed for high-voltage conditions.[32–37]
utilizing MXene as an excellent support material for various electrocatalysis. Transition metal carbides or nitrides or
carbonitrides of two-dimensional (2D) ma-
terials, also known as MXene (Mn+1 Xn Tx
(n = 1, 2, 3), M = early transition metal,
1. Introduction X = carbon and/or nitrogen, and Tx = surface functional groups,
such as ─O, ─OH, or ─F), are emerging as new candidates for
Water electrolysis has received much attention as an eco-friendly catalyst supports owing to their unique properties such as high
and carbon-neutral hydrogen production technology.[1–5] How- electrical conductivity, hydrophilicity, abundant surface func-
ever, its practical application to hydrogen stations and supply tional groups, and stability.[38–41] Although MXene has recently
chains has been hampered due to the sluggish kinetics of the been studied as an electrocatalyst for clean energy conversion
anodic oxygen evolution reaction (OER).[6–8] Accordingly, exten- reactions,[31,42–57] its practical use is rarely feasible due to the large
sive efforts have been made to develop novel OER electrocata- gap in reaching the catalytic activity levels of the related technolo-
lysts, such as Ru, Ir-based catalysts, metal oxides, metal sulfides, gies. Meanwhile, many studies have obtained promising results
and metal phosphides, with substantially improved OER kinetics when using MXene as the support material, including for OER
to enable the widespread application of water electrolyzers.[9–12] catalysts.[58–65]
While these advanced electrocatalysts have achieved better OER Previous review articles have focused on the properties,
activities, the limitations of elemental leaching or particle ag- applications, synthesis methods, and catalytic activities of
glomeration become apparent when utilized alone under high- MXene.[66–79] Some more reviews highlighted MXene as the
voltage conditions, severely degrading catalyst stability.[13–22] catalyst support for oxygen reduction reaction (ORR)[63,80,81]
and as support/hybrid catalysts for hydrogen evolution reac-
tion (HER).[64,65] While attempts have been made to incor-
B. R. Anne, J. Kundu, M. K. Kabiraz, J. Kim, D. Cho, S.-I. Choi
Department of Chemistry and Green-Nano Materials Research Center
porate the water-splitting performance of MXene-added cata-
Kyungpook National University lyst compounds, previous articles have presented the role of
Daegu 41566, Republic of Korea MXene as a hybrid catalyst or as a sole catalyst, and fur-
E-mail: sichoi@knu.ac.kr ther investigated defect-oriented MXene for enhanced catalytic
B. R. Anne properties.[69,71,74,82,83] However, within the existing literature,
Department of Metallurgical and Materials Engineering less emphasis has been placed on the role of MXene as a support
National Institute of Technology
Warangal 506004, India material for OER. Therefore, this review highlights the necessity
and emergence of coupling MXene support with OER catalysts.
The ORCID identification number(s) for the author(s) of this article From the perspective of utilizing MXene as a support material, we
can be found under https://doi.org/10.1002/adfm.202306100 introduce an OER mechanism and discuss the synergistic effect
DOI: 10.1002/adfm.202306100 on electrocatalysis between catalysts and MXene supports. We
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Figure 1. Adsorbate evolution mechanism (AEM) of OER a) in acidic media and b) in alkaline media. c) Lattice-oxygen mediated mechanism (LOM) of
OER. An active site and an oxygen vacancy denoted by M and ◻.
also summarize the synthesis methods of MXene and catalyst- Sabatier principle, the O-containing adsorbates should bind nei-
MXene compounds and detail the key properties of MXene as the ther too strongly nor too weakly to the surface of the catalysts.[94]
support to improve the OER performances. Finally, this article A typical AEM involves four concerted proton-electron trans-
provides challenges and future prospects for exploring research fer (CPET) reactions on a single metal center.[95,96] Acidic and
opportunities of MXene as the catalyst support for various energy alkaline media facilitate different reaction steps, as shown in
conversion reactions. Figure 1a,b.[6,97–100] The metal center acts as both the adsorption
site and redox center when the O2 p-band is positioned lower
than the metal d-band. In the first CPET step, the O-vacancy
2. Introduction of OER Mechanism metal surface (M) captivates the OH. In the second step, de-
protonation occurs to the M─OH, and later, M─OOH is gen-
The theoretical redox potentials of OER and HER at different erated by O─O bond formation between M─O and OH. Fi-
pH conditions are determined from the Nernst equation, assess- nally, deprotonation of M─OOH results in O2 evolution along-
ing the overall water-splitting efficiency. At pH 0, the OER po- side restituting the active M site. It should be noted that ─O,
tential is 1.23 V, and the HER potential is 0 V. At pH 7, the ─OH, and ─OOH adsorbates retain their own difference in
OER potential is 0.81 V, and the HER potential is −0.413 V. At the Gibbs free energy of adsorption (ΔG) during the reaction
pH 14, the OER potential is 0.4 V, and the HER potential is mechanisms.
−0.826 V.[84,85] Therefore, the overall potential for water split-
ting remains constant at 1.23 V at all pH conditions. Previous
research has shown that the OER is sluggish in all media and 2.2. Brief Introduction of LOM
dependent on specific reaction conditions. In acidic media, the
sluggishness of the OER is attributed to the four-electron/four- In this mechanism, direct O─O bonding with a reversible gen-
proton coupled steps and O-O bond formation.[86–88] The slug- eration of lattice oxygen vacancy (denoted by ◻) is affirmative
gish kinetics of OER in alkaline media is limited by the mul- due to bond weakening between metal cations and oxygen ow-
tistep process of the proton transfer.[89] In neutral electrolytes, ing to an increase in covalency (Figure 1c).[100] Generally, LOM
the OER mechanism has been suggested to be a proton-coupled is a pathway that originates from two neighboring metal sites, in
electron-transfer process, and the proton transfer can be slug- contrast to AEM, which predominantly occurs at a single metal
gish due to the low solubility of protons in neutral media.[90–92] site.[101] Initially, deprotonation occurs between M─OH and OH−
Since OER is a major cause of reducing the efficiency and perfor- species. Then, oxo-species are coupled to form an O─O bond
mance of water electrolysis, many studies have been conducted rather than creating M─OOH.[99,101] Lastly, O2 is released from
to improve the activity by understanding the mechanism.[6–8] Var- the metal surface, and the OOH is not involved in the catalytic
ious mechanisms have been proposed in this regard, and two cycle of LOM as an intermediate. This LOM has been a more ra-
mechanisms are now most plausibly accepted; adsorbate evo- tionally accepted process than AEM for transition metal-based
lution mechanism (AEM) and lattice-oxygen mediated mecha- catalysts.[99,101–103] Specifically, an oxygen vacancy is generated
nism (LOM). The two mechanisms are briefly described in this due to the electron transfer from the O2 p-band to the metal d-
section. band when the energy of the O2 p-band is higher than that of
the occupied metal d-band. Although LOM is considered as a
potential mechanism that could explain the evolution of O2 , it
2.1. Brief Introduction of AEM is relatively new and needs further experimental and theoreti-
cal validation.[8,53,104–108] For the MXene-supported OER catalysts,
In AEM for OER, it is widely accepted that the binding strength LOM studies have been very limited. Therefore, the following sec-
between the catalyst surface and O-containing adsorbates domi- tion only describes the AEM-based OER for the catalyst-MXene
nantly influences the reaction overpotential.[93] According to the compounds.
Figure 2. a) OER pathway in an alkaline medium. Free energy diagrams for overall OER pathway at an equilibrium potential of b) 0 V and c) 1.23 V in
H2 PO2 − /FeNi-LDH-V2 CTx . Reproduced with permission.[110] Copyright 2021, Elsevier B.V.
2.3. Impact of MXene Supports on OER Mechanism mended, as it enhances charge transfer kinetics and promotes ap-
propriate adsorption/desorption properties of the reaction inter-
Although the suggested mechanisms are helpful in understand- mediates, leading to higher OER activity in H2 PO2 − /FeNi-LDH-
ing the OER catalysis and developing better catalysts, it is chal- V2 CTx .[110]
lenging to attempt a mechanistic understanding of MXene with Consequently, understanding the OER mechanism helps in
its limited role as a support material. However, several results comprehending the role of catalysts, and a further improvement
suggesting a catalyst-support hybrid role of MXene have at- in the OER activity can be achieved by modifying the catalysts.
tempted to explain the M-OOH formation mechanism, namely Various methods are currently being employed to develop ad-
AEM. For example, post-OER analysis of CoP/Ti3 C2 Tx revealed vanced MXene-supported OER catalysts, highlighting the impor-
the transformation of CoP into 𝛽-CoOOH during OER catalysis. tance of the role of MXene in future studies.
The 𝛽-CoOOH was identified as the actual catalytic site, and the
formation of this phase favored the OER.[25] In addition, proper 3. Synthesis of MXene and Catalyst-MXene
bonding of the reaction intermediates to the catalyst surface was Compounds
observed, resulting in improved adsorption/desorption proper-
ties during OER on CoP/Mo2 CTx . The appropriate bond strength MXene is generally obtained from its precursor MAX phase
was attained through strong electronic coupling between CoP (Mn+1 AXn ), where M represents an early transition metal, A rep-
and Mo2 CTx , as confirmed by the negative shift in the d-band resents group 13 or 14 elements, and X represents carbon or ni-
center of CoP/Mo2 CTx than bare CoP.[109] In another study, Chen trogen. The MAX phase features a laminated structure in which
and co-workers obtained free energy diagrams for the overall an “A” monolayer is regularly sandwiched between Mn+1 Xn lay-
OER pathway at a given equilibrium potential using density func- ers. The unit cells of various types of MAX denoted as “211′, ‘312′,
tional theory (DFT) calculations in H2 PO2 − /FeNi-layered double and ‘413′ based on the layer numbers of M, A, and X are shown in
hydroxides (LDH)-V2 CTx . The results of the H2 PO2 − /FeNi-LDH- Figure 3a. The M-A bond is weaker and longer than the M-X bond
V2 CTx catalyst were compared with those of H2 PO2 − /FeNi-LDH. owing to the similar electronegativity between M and A.[111–113]
Figure 2a represents the reaction pathway of the OER, which Therefore, the ‘A” atomic layer can be eliminated through spe-
was utilized to construct the free energy diagram for the over- cific etching to synthesize MXene.[114]
all OER pathway. At an equilibrium potential of 0 V, the forma- MXene is a transition metal carbide/nitride, with common
tion of *OOH from *OH was the OER rate-determining step forms including M2 XTx , M3 X2 Tx , and M4 X2 Tx , where Tx de-
in both H2 PO2 − /FeNi-LDH-V2 CTx (1.56 eV) and H2 PO2 − /FeNi- notes surface functional groups, namely, ─O, ─OH, ─F. A MX-
LDH (1.69 eV), as shown in Figure 2b. The reduced free energy ene structure comprises three integral parts, and the first one
barrier in the H2 PO2 − /FeNi-LDH-V2 CTx suggested that the O-O is the intra-skeleton layer consisting of M and X atoms in alter-
bond formation energy is lowered after adding V2 CTx to the cat- nate layers stacked with ionic bonds. The second one is the inter-
alyst. This can be attributed to the strong electronic coupling be- skeleton domain, where the weak Van der Waals forces maintain
tween the catalyst and V2 CTx , which alters the electrophilicity of the attraction between layers among surface atoms (O/F) and the
the catalyst. At a potential of 1.23 V, ΔG*OH in H2 PO2 − /FeNi-LDH hydrogen bond between them. The last one is the Tx groups ran-
showed a negative value, indicating strong adsorption of *OH, re- domly positioned on the MXene surface.[115] The Tx groups can
sulting in a higher energy requirement for the formation of *O be modulated depending on various synthesis procedures. The
and *OOH intermediates (Figure 2c). On the contrary, the lower schematic of various MXene structures derived from the corre-
ΔG difference between reaction intermediates in H2 PO2 − /FeNi- sponding MAX precursors is shown in Figure 3b. Thus far, more
LDH-V2 CTx suggested an appropriate balance between adsorp- than 30 different types of MXene have been experimentally re-
tion and desorption, which is beneficial for OER kinetics. There- ported, with Ti3 C2 Tx accounting for over 70% of the identified
fore, the synergistic effect of V2 CTx and FeNi-LDHs was recom- MXene types.
Figure 3. a) Three different types of MAX unit cells: 211-M2 AX, 312-M3 AX2 , and 413-M4 AX3 . Reproduced with permission.[116] Copyright 2016, Elsevier.
B. V. b) Schematic structure of M2 XT2 , M3 X2 T2 , and M4 X3 T2 MXene derived from their respective MAX precursors. Reproduced with permission.[117]
Copyright 2018, Elsevier Inc.
In the following subsections, we briefly introduce represen- In alkali etching, the formation of metal oxides or oxyhydrox-
tative synthesis methods of MXene that have enabled the effec- ides during alkali treatment makes it complicated, where the for-
tive etching of the “A” layer. Subsequently, we summarize various mation of such phases hinders the complete etching of “A” layers
preparation methods for catalyst-MXene compounds. in MAX.[139–142] In general, high temperature, pressure, and con-
centrated alkali solutions are involved in alkali etching to elimi-
nate (oxide) hydroxides. Zhang and co-workers successfully ob-
tained Ti3 C2 Tx (T = O, OH) with a purity of 92 wt% by prefer-
3.1. Synthesis Methods of MXene entially removing Al from Ti3 AlC2 at 270 °C in 27.5 M NaOH
(Figure 4e).[135] In another work, multi-layered Ti3 C2 (OH)2 was
As referred above, MXene is typically synthesized from MAX, obtained at 180 °C for 24 h using KOH etching with Ti3 AlC2 to
and various approaches have been explored to achieve this. To KOH ratio of 1:3.5. Later, monolayer Ti3 C2 (OH)2 was obtained
date, acid etching, alkali etching, electrochemical etching, and by the exfoliation with water.[140] Alkali etching poses fewer haz-
non-aqueous etching have been utilized for MXene synthesis. ards than HF etching, but using high temperatures, pressures,
Among these methods, acid etching or HF etching is the most and higher concentrations raises other safety concerns. In addi-
vastly used method to preferentially eliminate the “A” layer in tion, preventing corrosion of Ti3 C2 under concentrated alkaline
MAX using concentrated HF.[118–127] Barsoum and co-workers condition remains a challenge.
synthesized the first MXene (Ti3 C2 Tx ) by reacting Ti3 AlC2 MAX Electrochemical etching has been reported as an efficient
with 50% concentrated HF for 2 h at room temperature, fol- method for synthesizing MXene that is difficult to obtain by
lowed by ultrasonication with methanol to obtain a few layered other methods. For instance, V2 CTx was obtained by the etch-
Ti3 C2 Tx (Figure 4a).[128] Figure 4b,c shows Ti3 C2 Tx after HF ing method at 50% HF concentration for 48 h, and there was no
treatment and exfoliation, respectively. Also, increased interlayer etching method to synthesize Cr2 CTx . However, both V2 CTx and
spacing among Ti3 C2 Tx sheets after sonication was confirmed Cr2 CTx were synthesized in a short time via electrochemical etch-
by HRTEM (Figure 4d). The mechanism of acid etching includes ing under relatively mild 1 M HCl conditions at an etching tem-
the reactivity between HF and Ti3 AlC2 MAX, where Al atoms are perature of 50 °C, with the potential varied to 0.5 V for V2 CTx
removed by forming AlF3, and the MXene is functionalized with and 1 V for Cr2 CTx , respectively.[143] Unlike chemical etching,
─F and ─OH to obtain a stable 2D structure. Few layered MXene electrochemical etching occurs by direct charge transfer from the
sheets can be further obtained by exfoliation, typically performed target to another substance. For example, electrochemical corro-
under ultrasonication with cationic surfactants such as tetram- sion at 5 V and room temperature for 5 h was utilized to ob-
ethylammonium hydroxide (TMAOH), tetrabutylammonium hy- tain Ti3 C2 Tx (T = O, OH). The cell configuration and etching
droxide (TBAOH), and dimethyl sulfoxide (DMSO). Despite the mechanism are given in Figure 4f, where two Ti3 AlC2 electrodes
effectiveness of this etching method, several drawbacks remain, were configured as the cathode and anode in a mixture of 0.1 M
including its limited applicability to non-Al-based MAX phases, NH4 Cl and 0.2 M TMAOH electrolyte. Figure 4g,i shows the SEM
limited applications of ─F terminated MXene, lower stability, in- images of Ti3 AlC2 and Ti3 C2 Tx before and after electrochemi-
ferior electrochemical properties, and concerns regarding chem- cal etching, respectively, revealing the tightly stacked MXene lay-
ical safety.[52,54,129–134] Therefore, enormous efforts have been in- ers after etching. Increased interlayer spacing from 17.08 ± 0.8
vested in originating alternative methods for synthesizing F-free Å (Ti3 AlC2 ) to 21 ± 2.5 Å (Ti3 C2 Tx ) after etching was observed
MXene. from HRTEM images (Figure 4h,j).[136] Electrochemical etching
Figure 4. a) Schematic of acid etching mechanism, and TEM images of b) exfoliated Ti3 C2 Tx (the inset showing the SAED pattern of hexagonal sym-
metry), and c) single and double-layered Ti3 C2 Tx nanosheets. d) HRTEM image of Ti3 C2 Tx nanosheets. Reproduced with permission.[128] Copyright
2011, Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim e) Alkali etching of Ti3 AlC2 by aqueous-NaOH solution at different conditions. Reproduced
with permission.[135] Copyright 2018, Wiley-VCH Verlag GmbH & Co. f) Schematic of electrochemical etching process, SEM and HRTEM images of
g,h) Ti3 AlC2 and i,j) Ti3 C2 Tx before and after etching. Reproduced with permission.[136] Copyright 2018, Wiley-VCH Verlag GmbH & Co. KGaA, Wein-
heim. k) Molten-salt etching mechanism of Ti3 SiC2 with CuCl2 . Reproduced with permission.[137] Copyright 2020, Springer Nature Ltd. l) Mechanism
of Iodine-assisted etching. Reproduced under the terms of the CC-BY-NC-ND license.[138] Copyright 2021, Wiley-VCH Verlag GmbH & Co.
enables environmental-related safety through optimized elec- the MAX. For instance, they added molten CuCl2 to Ti3 SiC2 and
trolyte selection. Therefore, electrochemical etching has the po- heated them at 750 °C for 7 h under Ar to produce Ti3 C2 Cl2 . The
tential to become a generalized method for rapid and facile syn- proposed etching mechanism is given in Figure 4k. Based on the
thesis of MXene with minimal toxicity. redox-potential rule, various MAX (Ti2 AlC, Ti3 AlC2 , Ti3 AlCN,
Till now, Lewis acidic molten salt etching and iodine (I2 )- Ti2 ZnC, Ti3 ZnC2 , Ta2 AlC, and Nb2 AlC) were practiced to obtain
assisted etching have been utilized in non-aqueous etching their corresponding MXene by treating with Lewis acidic salts
methods. Huang and co-workers proposed the use of Lewis acidic such as NiCl2 , FeCl2 , CuCl2 , AgCl, CoCl2 , and CdCl2 .[137]
molten salts as effective oxidizing agents for the A-layer atoms in Moreover, molten-salt etching facilitated terminal group
Figure 5. a) Schematic representation of IrCo/ac-Ti3 C2 Tx synthesized by wet-chemical route. TEM images of b) HF-etched Ti3 C2 Tx , c) ac-Ti3 C2 Tx , and
d) uniformly distributed IrCo hollow structure on ac-Ti3 C2 Tx . Reproduced with permission.[145] Copyright 2019, Wiley-VCH Verlag GmbH&Co KGaA,
Weinheim. e) Schematic of preparing Co3 O4 /Ti3 C2 Tx by solvothermal route. f) TEM image of HF-etched Ti3 C2 Tx , g) SEM image of non-uniform pris-
tine Co3 O4 NPs, and h) TEM image of uniformly distributed Co3 O4 NPs on Ti3 C2 Tx . Reproduced with permission.[146] Copyright 2019, Elsevier B.V.
and Science China Press. i) Schematic of preparing CoP/Mo2 CTx by phase-transformation. SEM images of j) pristine Mo2 CTx , k) pristine CoP, and
l) CoP/Mo2 CTx . Reproduced with permission.[109] Copyright 2021, The Royal Society of Chemistry. m) Schematic of NiFe-LDH/Ti3 C2 Tx /NF preparation
by electrodeposition. SEM images of n) microporous scaffold of NiFe-LDH/Ti3 C2 Tx /NF electrode (the inset showing optical image of the scaffold with
an area of 70 cm2 ) and o) mesoporous network of NiFe-LDH nanosheets on Ti3 C2 Tx /NF frame. TEM images of p) NiFe-LDH/Ti3 C2 Tx and q) amorphous
texture of NiFe-LDH nanosheets. Reproduced with permission.[147] Copyright 2019, Elsevier Ltd.
transformation and defect creation on the MXene surface.[144] tioned in Section 3.1. The firm fixation of the catalyst onto the
Therefore, molten-salt etching can serve as an efficient way to MXene surface is of great importance in preparing the com-
modify the MAX and obtain F-free MXene. pounds. In addition, the morphology of the catalysts can be
In I2 -assisted etching, Ti3 C2 Ix with oxygen-rich terminal determined by the synthesis process. This section summarizes
groups was obtained by reacting Ti3 AlC2 with I2 in anhydrous several methods, including wet-chemical, phase-transformation,
acetonitrile at 100 °C for 4 days. The mechanism involved in the and electrodeposition to effectively prepare catalyst-MXene com-
I2 -assisted etching was the removal of Al atoms by forming AlI3 pounds.
particles (Figure 4l).[138] Although I2 -assisted etching requires a The wet-chemical method is widely adopted for anchoring
longer etching time than molten-salt etching, it needs lower en- catalysts or precursors (later converts into actual catalyst by
ergy consumption as it requires low operational temperatures. In phase-transformation) onto the surface of MXene. For exam-
addition, MXene produced through I2 -assisted etching often has ple, a facile wet-chemical method was utilized for synthesizing
higher purity and crystallinity than molten-salt etching. IrCo hollow structure on porous Ti3 C2 Tx . Firstly, Ti3 C2 Tx was
obtained from Ti3 AlC2 by HF etching. Later, activated porous
Ti3 C2 Tx (ac-Ti3 C2 Tx ) was obtained by treating HF-etched Ti3 C2 Tx
3.2. Preparation of Catalyst-MXene Compounds with a mixture of HCl and H2 O2 . Then, IrCo hollow structures
were attached to ac-Ti3 C2 Tx by wet-chemical synthesis method.
Various catalysts have been synthesized on different types of MX- Schematic of the synthesis protocol is shown in Figure 5a.
ene after obtaining the MXene using any of the approaches men- Figure 5b,c shows the TEM images of HF-etched Ti3 C2 Tx and
ac-Ti3 C2 Tx , respectively, indicating abundant holes at basal employed the electrodeposition method to deposit NiFe-LDH on
planes and edges (yellow circles) in ac-Ti3 C2 Tx . For the synthesis Ti3 C2 Tx , and the synthesis schematic is given in Figure 5m.[147]
of IrCo hollow structure on ac-Ti3 C2 Tx , a mixture of IrCl2 .xH2 O Ti3 C2 Tx was synthesized using acid etching with a solution mix-
and Co(NO3 )2 .6H2 O with 1:5 molar ratio was prepared by dis- ture of LiF and HCl at 35 °C for 24 h. In this study, NF served
solving them in deionized water and kept the solution for 2 h at as a substrate for NiFe-LDH/Ti3 C2 Tx , and Ti3 C2 Tx was coated
room temperature. Later, this mixture was added to ac-Ti3 C2 Tx on NF by soaking NF in an aqueous suspension of Ti3 C2 Tx for
suspension and heated at 60 °C for 1 h. Then, KBH4 solution 30 min. The electrostatic interaction between the electronegative
was added to the mixture and treated for 12 h to obtain IrCo@ac- MXene and positively charged NF led to the formation of a 3D
Ti3 C2 Tx . Figure 5d shows the uniformly dispersed IrCo hollow microporous scaffold of Ti3 C2 Tx /NF. Later, NiFe-LDH was elec-
structure on porous ac-Ti3 C2 Tx without agglomeration. The ac- trodeposited using a three-electrode system, with Ti3 C2 Tx /NF,
Ti3 C2 Tx with a highly porous structure, huge specific surface area Pt foil, and Ag/AgCl serving as working, counter, and reference
(SSA), and a greater number of edges/defects provided a max- electrodes, respectively. An aqueous solution consisting of nickel
imal and uniform distribution of IrCo. Moreover, IrCo hollow nitrate and ferrous nitrate was used as the electrolyte. Various
structure prevented the re-stacking of MXene layers. Thus, pre- NiFe-LDH/Ti3 C2 Tx /NF electrodes were fabricated by controlling
vented re-stacking of MXene and agglomeration of IrCo facili- the deposition potential (−0.8 to −1.2 V), the deposition time
tated higher exposed area to the electrolyte during electrocatalytic (60–360 s), and the molar ratio of Ni:Fe (1:3 to 4:0). The de-
reactions.[145] posited NiFe-LDH adopted the interconnected 3D structure of
A solvothermal method is also applied to affix nanocatalysts the Ti3 C2 Tx /NF frame without blocking macropores (Figure 5n).
on the MXene surface. For example, Lu and co-workers prepared Amorphous NiFe-LDH nanosheets formed a dense network,
Co3 O4 nanoparticles (NPs) on the surface of Ti3 C2 Tx by solvother- ≈100–130 nm thick, along with the mesopores in the range of
mal method. First, Ti3 C2 Tx was obtained by HF etching. Then, tens of nanometers between the NiFe-LDH and the Ti3 C2 Tx sur-
Ti3 C2 Tx powder was added to the cobalt acetate solution of 30 mL face, as shown in Figure 5o–q. This kind of structural feature is
anhydrous ethanol and treated at 80 °C for 10 h under N2 flow. beneficial in exposing more edge and defect sites and shortening
The mixture was transferred to a Teflon-lined stainless-steel au- the charge transport path during electrocatalytic reactions.
toclave and heated at 150 °C for 3 h to produce Co3 O4 /Ti3 C2 Tx . The catalyst-MXene compounds synthesized in these ways fa-
Figure 5e represents the schematic of the synthesis procedure vor electrochemical reactions due to the strong electronic cou-
of Co3 O4 /Ti3 C2 Tx catalyst. Figure 5f shows the TEM image of pling between the catalyst and MXene. The synergistic effect be-
pristine Ti3 C2 Tx with few-layered nanosheets. Non-uniform par- tween the catalyst and MXene is discussed in the following sec-
ticle size and aggregated pristine Co3 O4 NPs before introduc- tions.
ing Ti3 C2 Tx are shown in Figure 5g. Much smaller particle size
and more uniform distribution of Co3 O4 NPs were confirmed
after adding Ti3 C2 Tx as a support (Figure 5h), which benefitted 4. Role of MXene as a Support Material
the charge transfer from Co3 O4 NPs to Ti3 C2 Tx during the OER
process.[146] Throughout the catalytic process, the catalyst support not only
Metal phosphide, nitride, and a few sulfide-based catalysts acts as a solid support but also helps in intensification and ut-
were anchored on MXene by a phase-transformation through most utilization of catalytically active sites. Moreover, the catalyst
solid-state reaction. Phase-transformation approach involves support implicitly contributes to the catalytic activity by increas-
conversion of respective precursor phase into the actual catalyst ing the charge transfer kinetics of the catalyst.[25,27,28,148] There-
phase. For example, Tian and co-workers prepared CoP/Mo2 CTx fore, the supporting materials for electrocatalysis should contain
catalyst compound using phase-transformation approach. At several crucial properties: i) prevention of catalyst aggregation by
first, Mo2 CTx was obtained by HF etching of Mo2 Ga2 C at 55 °C improving SSA; ii) a high conductivity facilitating electron trans-
for 160 h.[109] Then, Co(OH)F/Mo2 CTx precursor was synthe- fer between the catalyst and the support material; iii) improving
sized using a hydrothermal route, represented in Figure 5i. the electronic properties of metal catalyst through SMSI; and iv)
Later, a solid-state reaction was carried out for the mixture of good electrochemical stability under redox conditions.[32,149–152]
Co(OH)F/Mo2 CTx and NaH2 PO2 at 350 °C for 2 h in Ar atmo- Additional requirements for efficient catalyst support include
sphere to obtain the final catalyst, CoP/Mo2 CTx . SEM images a suitable porous structure, electrode compatibility, and good
of bare Mo2 CTx and CoP are shown in Figure 5j,k, respectively. hydrophilicity.[153]
Dense growth of CoP on Mo2 CTx surface occurred after phase- Novel 2D MXene has attracted significant interest as catalyst
transformation of the Co(OH)F, as shown in Figure 5l. This supports owing to the distinctive properties of large surface area,
work also confirmed the existence of macro and mesopores in high electrical conductivity, SMSI, and long-term stability, as in-
CoP/Mo2 CTx catalyst by determining the pore size distribution troduced above, along with the additional feature of hydrophilic-
with an average pore size of 1.7–11.8 nm. Further, SSA of the CoP ity. More exceptionally, the higher redox activity than carbona-
catalyst (7.96 m2 g−1 ) increased to 46.49 m2 g−1 (CoP/Mo2 CTx ) af- ceous supports owing to the terminal groups on the MXene sur-
ter adding MXene. It was suggested that such highly porous with face has made it interesting to investigate MXene as a support
a large surface area may favor ion and mass transportation dur- material.[154,155] Due to these unique physical and chemical prop-
ing electrocatalytic reactions. erties, multi-functional MXene has great potential for catalytic
Electrodeposition method was vastly utilized as the second application as supporting materials for OER and other energy
most common technique, after wet-chemical synthesis, to anchor conversion technologies. This section describes the significance
catalysts on the MXene support. For example, Qiu and co-workers and key properties of MXene as catalyst supports.
4.1. Prevention of Aggregation and Restacking of Catalyst-MXene coupling between the catalyst and MXene.[134] Due to its high
Compounds electronegativity, MXene spontaneously attracts electrons from
the catalyst, resulting in a rapid charge transfer between the cat-
Previous literature has shown that the 2D/3D conductive net- alyst and MXene. For example, 0.44 electrons per formula unit
work of MXene not only withstands volume expansion but (f.u.) were transferred from the NiFeP catalyst to Ti3 C2 Tx . In ad-
also prevents the agglomeration of NPs during nanocata- dition, changes in the electronic structure of NiFe-LDH/Ti3 C2 Tx
lyst synthesis.[156–159] This flexibility of MXene nanosheets has and NiFeP/Ti3 C2 Tx were assessed in comparison with bare NiFe-
gained research interest in preparing the nanocatalysts on LDH by calculating the density of states (DOS) and projected
the surface of MXene, allowing them to increase the SSA DOS (PDOS). The DOS analysis around the Fermi energy level
of the catalyst, which is beneficial for electrocatalytic activity. revealed the enhanced electrical conductivity of the catalyst-
For example, Huang and co-workers synthesized 2D porous MXene compounds, indicating the metallic nature (Figure 6a).
cobalt 1,4-benzenedicarboxylate (CoBDC) catalyst on 2D Ti3 C2 Tx Also, PDOS of 3d orbitals for Ni and Fe in bare NiFe-LDH and
nanosheets as an effective OER catalyst.[160] In this case, Ti3 C2 Tx NiFeP/Ti3 C2 Tx demonstrated a positive shift in the d-band cen-
nanosheets prevented the aggregation of the CoBDC catalyst dur- ters of Ni and Fe atoms in NiFeP/Ti3 C2 Tx (−2.24 eV) compared
ing the synthesis process, thereby increasing the exposure of the to bare NiFe-LDH (−2.61 eV), as shown in Figure 6b. This in-
porous structure to the electrolyte by improving the SSA. As a creased d-band center reduces the electronic filling of the anti-
result, CoBDC catalyst exhibited an initial SSA of 106.6 m2 g−1 , bonding state, resulting in improved bonding strength between
which improved to 199.1 m2 g−1 after adding Ti3 C2 Tx . In another NiFeP/Ti3 C2 Tx surface and intermediates. It is widely accepted
study, Hu and co-workers fabricated a vertical array structure of that the accumulation of charge carriers and enhanced electrical
CoFe-LDH on Ti3 C2 Tx , effectively preventing the aggregation of conductivity are associated with improved OER activity.[27]
CoFe-LDH and thus providing a higher SSA.[161]
Peng and co-workers investigated another crucial point of pre-
venting the restacking of Ti3 C2 Tx sheets by introducing CoS2 be- 4.4. Stability
tween MXene sheets.[162] The isolated MXene sheets provided
more anchored sites for the active CoS2 catalyst. As discussed The surface of MXene layers is chemically stable, with C-
above, MXene played a vital role in preventing the aggrega- containing MXene being more chemically stable than the N-
tion of CoS2 catalyst, as confirmed by the enhanced SSA of the containing MXene.[65] Moreover, the dynamic stability of the
CoS2 /Ti3 C2 Tx (46.2 m2 g−1 ), where the pristine CoS2 and Ti3 C2 Tx MXene is usually controlled by the surface functional groups.
exhibited SSAs of 6.4 m2 g−1 and 15.1 m2 g−1 , respectively. For example, ─OH group easily decomposes, while ─F group
is often prone to desorption or replacement by other elements
due to weak chemical bonding.[54] However, MXene with the
4.2. Electrical Conductivity
─O terminal group is the most stable, as the inner transition
metal atoms are protected from environmental exposure by the
MXene has higher electrical conductivity when compared with
─O group, improving the oxidation resistance and stability of
other 2D materials such as graphene, where the maximum re-
MXene.[169] This is particularly beneficial in highly corrosive
ported electrical conductivity of graphene is 10 000 S cm−1 ,[163]
working environments such as water electrolysis.[170] Further-
while Ti-based-MXene has demonstrated conductivity up to
more, catalyst materials for long-term applications should have
24 000 S cm−1 .[164,165] It should be noted that the electrical con-
high durability without sacrificing catalytic activity. In this re-
ductivity of MXene can be adjusted from metallic to semicon-
spect, the electrocatalysts hybridized with MXene have demon-
ducting or even insulating by controlling the compositions of
strated better stability without substantial degradation or chem-
“M,” “X,” and “T” in MXene.[166] In addition, the change in con-
ical reactions in alkaline and acidic conditions.[25,171,172] For ex-
ductivity of MXene is attributed to several aspects: i) termination
ample, NiFeLa-LDH/vertically aligned Ti3 C2 Tx (v-Ti3 C2 Tx )/NF
group; ii) delamination yield; iii) the number of defects; iv) the
exhibited excellent stability up to 1200 h at a current density
lateral size of MXene flakes, and v) the d-spacing between MX-
of 100 mA cm−2 in 1.0 M KOH, outperforming commercial
ene layers.[167] Therefore, highly conducting MXene with opti-
RuO2 /NF that showed a drastic potential rise beyond 100 h.[173]
mal compositions can be a suitable candidate for catalyst sup-
Likewise, MXene-supported OER catalysts demonstrated higher
port owing to their enhanced charge transfer across the cata-
stabilities due to the strong synergy between catalyst and MXene.
lysts. For example, pristine FeNi-LDH and FeNi-LDH-reduced
The higher chemical and structural stability of MXene works syn-
graphene oxide (rGO) catalysts demonstrated charge transfer re-
ergistically with improved charge transfer and strong interfacial
sistance (Rct ) of 24.7 and 10 Ω, respectively. On the contrary, the
and electronic coupling between catalyst and MXene, contribut-
addition of Ti3 C2 Tx to FeNi-LDH (FeNi-LDH/Ti3 C2 Tx ) resulted
ing to the better structural stability of the catalyst-MXene com-
in a reduced Rct of 5.1 Ω. The electrochemical impedance spec-
pounds.
troscopy (EIS) profile also showed enhanced charge transfer of
FeNi-LDH/Ti3 C2 Tx .[19]
4.5. Hydrophilicity
4.3. SMSI
Hydrophilicity is another specific property of MXene for applica-
The surface functionality of MXene alters the electronic struc- tion as a catalyst support. MXene exhibits excellent hydrophilic-
ture of the catalyst, creating a strong electronic and interfacial ity due to its abundant surface functional groups (F/O/OH/Cl).
Figure 6. a) DOS of NiFe-LDH/Ti3 C2 Tx and NiFeP/Ti3 C2 Tx compared with bare NiFe-LDH. The dashed line indicating the Fermi level. b) PDOS of 3d
orbitals in NiFeP/Ti3 C2 Tx and bare NiFe-LDH. The dashed lines indicating the d-band centers in each case. Reproduced with permission.[27] Copyright
2021, Science China Press. The contact angles (CA) of the 1.0 M KOH droplets on c) NF, d) Ti3 C2 Tx /NF, e) NiFe-LDH/NF, and f) NiFe-LDH/Ti3 C2 Tx /NF
electrodes. Reproduced with permission.[168] Copyright 2020, Elsevier Inc.
It is also accepted that the various functional groups of MX- 4.6. Advantages of MXene Supports Over Other Supports
ene determine the hydrophilicity of MXene. This unique hy-
drophilicity of MXene can be correlated to the OER performance This section highlights the advantages of MXene supports over
of catalyst-MXene compounds. For example, Wu and co-workers other existing support materials and explains the favorable tun-
measured the hydrophilicity of the catalyst-MXene compound ing of MXene properties based on chemical structure. MX-
by measuring the contact angle for NiFe-LDH/Ti3 C2 Tx /NF.[168] ene supports have better electrochemical stability and greater
The hydrophilicity of NiFe-LDH/Ti3 C2 Tx /NF was compared with corrosion resistance than carbon-based supports. For example,
NF, Ti3 C2 Tx /NF, and NiFe-LDH/NF. The contact angle of the Pt, supported on carbon, showed poor ORR stability compared
NiFe-LDH/Ti3 C2 Tx /NF interface was ≈0° (Figure 6f), indicating to the Pt/MXene catalyst in corrosive acidic environments.[142]
its hydrophilic nature. The NF, Ti3 C2 Tx /NF, and NiFe-LDH/NF Also, NiFe-LDH/Ti3 C2 Tx /rGO showed higher OER stability than
interfaces demonstrated contact angles of 119.7° (Figure 6c), 0° NiFe-LDH/rGO after a 4 h chronopotentiometric test at a cur-
(Figure 6d), and 86.2° (Figure 6e), respectively. Higher interac- rent density of 10 mA cm−2 in 1.0 M KOH solution, where
tions between the catalytically active sites and water molecules NiFe-LDH/rGO suffered severe degradation.[178] In addition, MX-
could increase the adsorption of oxygen molecules, which would ene is significantly more hydrophilic than NF, carbon-based
benefit OER performance.[174–177] Understanding the detailed supports (carbon black, carbon paper, glassy carbon, graphene,
mechanism of hydrophilicity of catalyst-MXene compounds to- graphdiyne), boron nitride (BN), and transition metal dichalco-
ward the OER activity requires further investigations. genides (TMDs).[147,173,179–187] Therefore, the hydrophilicity of
catalysts can be controllable by adding or removing MXene. For 5. OER Performances

example, the hydrophilicity of NiFe-LDH catalyst was improved
after Ti3 C2 Tx addition, while the hydrophobicity increased in the Although the OER activity of pristine MXene is rarely available,
absence of Ti3 C2 Tx .[168,173] many studies confirmed that MXene is suitable support mate-
Although MXene and 2D graphene-based supports show high rial for OER electrocatalysts. This section discusses the improved
conductivity, MXene-supported catalysts exhibit faster charge OER performances of catalyst-MXene compounds concerning
transfer kinetics compared to rGO-supported catalysts. This is be- the role of MXene. In addition, the content is organized into sev-
cause the properties of MXene can be favorably altered by func- eral subsections according to the representative class of materi-
tionalizing, alloying, and changing its chemical composition to als.
form stronger interfacial and electronic coupling between the cat-
alyst and MXene support.[188] For example, FeNi-LDH/Ti3 C2 Tx 5.1. LDHs-Structured Catalysts Coupled with MXene Supports
showed 4.8 times lower Rct than FeNi-LDH/rGO.[19] In addition,
poor conductivity poses a key challenge for oxide-based supports, LDHs can exhibit good OER activity because their 2D layered
which can be improved by introducing MXene.[189–191] For exam- nanostructures are composed of cationic nanosheets intercalated
ple, FeNi-LDH/Ti3 C2 Tx /TiO2 showed higher charge-transfer ki- with anionic species and many active sites. However, the long-
netics than FeNi-LDH/TiO2 , thereby enhancing OER activity of term performance of LDHs is limited by their aggregating na-
the FeNi-LDH/Ti3 C2 Tx /TiO2 .[192] ture and poor conductivity.[199] To overcome these issues, con-
Unlike other catalyst supports, the properties of MXene ductive supports can be utilized to anchor LDHs. For example,
can be easily tuned by changing terminal groups, inter-layer Ti3 C2 Tx inhibited the aggregation of FeNi-LDH. The improved
distance, and chemical composition.[167] For example, Mo- SSA of FeNi-LDH/Ti3 C2 Tx compared to the pristine FeNi-LDH
based MXene, including ─OH and ─F groups, behaved like a is one of the indications for aggregation prevention. The uni-
semiconductor, whereas O-terminated MXene showed metallic formly distributed FeNi-LDH with a loosely packed porous net-
nature.[167,193] Moreover, the electronic structure of the catalyst- work of very thin nanoplates on Ti3 C2 Tx is shown in Figure 7a.
MXene can be easily altered by termination groups with high Such ultrathin and porous structured morphology was attributed
electronegativity, which helps in achieving strong electronic to the shortened pathways for mass and electron transfer dur-
and interfacial coupling between the catalyst and MXene.[134] ing electrocatalysis. Moreover, SMSI reduced the potential bar-
For example, the high electronegativity of MXene attracted rier for charge transfer in FeNi-LDH/Ti3 C2 Tx . The DOS cal-
the electrons from the catalyst, which tunes the electronic culations of FeNi-LDH/Ti3 C2 Tx also evidenced synergistic elec-
structure and electrophilicity of catalytic active sites. This re- tronic interaction due to elevated charge transfer between FeNi-
sults in shifting the d-band center of the catalyst to the val- LDH and Ti3 C2 Tx compared to FeNi-LDH (Figure 7b). Typi-
ues close to the Fermi level in catalyst-MXene compounds, cally, the OER benefitted from the moderate binding strength
which was confirmed by the DOS and PDOS calculations by of intermediates. According to PDOS observations, the d-band
DFT.[27,28,109,110,148,161,194–197] The d-band center shift optimizes the center of Ni/Fe shifted to the more negative side in the FeNi-
adsorption/desorption properties of intermediates and thus en- LDH/Ti3 C2 Tx hybrid compared with bare LDH (Figure 7c). This
hances the OER activity. High electron mobility during electronegative shift explains the reduced binding strength of interme-
catalytic applications is associated with the functional groups diates on the surface of the catalyst during the OER process,
in MXene, indicating the favorable tuning of charge transfer ascribed to the strong electronic interaction among FeNi-LDH
through the modification of surface terminal groups.[198] There- and Ti3 C2 Tx . Due to the above-mentioned reasons, the FeNi-
fore, MXene can be a potential support material with inherent LDH/Ti3 C2 Tx showed an overpotential of 298 mV at a current
and combinatory properties of conductivity, hydrophilicity, and density of 10 mA cm−2 in 1.0 M KOH solution, the lowest among
stability. the compared catalysts, as shown in Figure 7d,e. Compared to
Further exploration is essential to resolve the complex mech- other 2D material supports, FeNi-LDH/Ti3 C2 Tx demonstrated
anisms linking catalysts and MXene supports, despite the re- faster charge transfer with the lowest Rct of 5.1 Ω, surpassing
markable electrocatalytic performances they display. Extensive FeNi-LDH/rGO (10 Ω) and FeNi-LDH (24.7 Ω). The improved
investigations have already shed light on key factors contribut- charge transfer is fundamentally associated with the tuned elec-
ing to the outstanding catalytic activity of MXene-based sup- tronic structure of the catalyst by adding MXene. Furthermore,
ports, including the electronic band structure and surface prop- the negatively charged ─OH and ─F groups on the MXene fa-
erties of MXenes. However, a comprehensive understanding of cilitated a strong interaction between FeNi-LDH and Ti3 C2 Tx .
the fundamental mechanisms driving the coupling strength and Thus, the long-term OER stability of FeNi-LDH improved after
enhanced electron transfer between MXenes and catalyst parti- adding Ti3 C2 Tx , as shown in Figure 7f.[19] This approach of in-
cles remains crucial. Moreover, MXene supports exhibit excep- corporating highly conductive MXene was also extended to other
tional stability in harsh catalytic environments, although the de- LDHs such as CoFe and CoNi.[161,195] The better OER activity of
bate surrounding their stability in aqueous environments per- LDH-MXene compound was due to immediate charge transfer
sists. Therefore, an in-depth investigation is required to reveal the between LDH and MXene that causes more positive charge cor-
underlying mechanism responsible for the increased stability of responding to Ni/Fe/Co centers in LDH that further promotes
MXene-catalyst compounds. Additionally, a thorough examina- electrostatic absorption of more anionic intermediates. More-
tion is necessary to clarify the complicated interactions among over, the presence of MXene enhanced the valence state of Ni2+
catalysts, MXene supports, and other secondary supporting into Ni3+,4+ . Besides high conductivity, MXene also assists in elec-
materials. tron extraction from LDHs. As a result, the d-band center of the
Figure 7. a) TEM image of FeNi-LDH/Ti3 C2 Tx , b) DOS of different catalysts, and c) PDOS of the Ni and Fe 3d orbitals from different catalysts, d) LSV
curves of different catalysts in 1.0 M KOH solution with a scan rate of 10 mA s−1 at 1600 rpm, e) OER overpotentials (𝜂 0 , 𝜂 10 ) of FeNi-LDH/Ti3 C2 Tx
in comparison with different catalysts, f) Chronopotentiometric performance of different catalysts at a constant current density of 10 mA cm−2 . Repro-
duced with permission.[19] Copyright 2017, Elsevier Ltd. SEM images of g) NiFeLa-LDH/v-Ti3 C2 Tx /NF and h) uniform distribution of NiFeLa-LDH on
v-Ti3 C2 Tx /NF, i) Polarization curve at a scan rate of 10 mv s−1 , j) Tafel plot, k) TOFs at different overpotentials, and l) Chronopotentiometric study at
100 mA cm−2 of NiFeLa-LDH/v-Ti3 C2 Tx /NF in comparison with different catalysts. All the electrochemical experiments were carried out in O2 saturated
1.0 M KOH solution. Reproduced with permission.[173] Copyright 2022, Elsevier B.V. and science press.
Ni/Fe/Co atoms shifts to the higher energy states, benefitting the alyst after adding MXene was confirmed by the stability test
appropriate binding strength of intermediates and redox OER at a constant overpotential and cyclic stability test without ap-
activity.[19,110,178,192,200,201] parent changes in current density and LSV curve, respectively.
Addressing the challenge of MXene sheet restacking, The improved OER performance of Co4 MnFe3 /Ti3 C2 Tx was as-
Zheng and co-workers transformed the 2D MXene into a signed to several advantageous aspects: (i) provision of more ac-
3D structure.[173] They developed hierarchical NiFeLa-LDH tive sites by increasing the disorder of Co4 MnFe3 surface owing
on vertically aligned 3D Ti3 C2 Tx (v-Ti3 C2 Tx ), where v-Ti3 C2 Tx to the incorporation of functional groups. (ii) improved stabil-
was electrodeposited on NF substrate. NiFeLa-LDH catalyst ity of Co4 MnFe3 /Ti3 C2 Tx due to conductive substrate and verti-
was uniformly distributed on the MXene layers by adapting cally aligned Co4 MnFe3 layers, creating 3D heterostructures. (iii)
the 3D porous structure (Figure 7g,h). This robust and porous enhanced charge transfer resulting from the synergy between
3D structure facilitates abundant open channels for electrolyte Co4 MnFe3 and Ti3 C2 Tx .[196]
access, favoring ion and mass transport during electrochemical OER activities of LDHs/LTHs catalysts supported by MXene
reactions. Also, strong electronic coupling between MXene and benefitted from the synergy between plentiful active sites from
LDH created a less occupied antibonding state between LDH LDHs/LTHs and conductive, hydrophilic MXene with strong in-
and absorbed O intermediates. This promotes the maintenance terfacial and electronic coupling resulting in lower overpotentials
of appropriate O-binding strength, thus increasing the OER and Tafel slopes are enlisted in Table 1.
activity of the material. NiFeLa-LDH/v-Ti3 C2 Tx /NF electrode
showed the best OER activity (overpotential = 191 mV) among all
the compared catalysts because of the robust surface morphol- 5.2. Metal Oxide Catalysts on MXene Supports
ogy and SMSI (Figure 7i–k). The NiFeLa-LDH/v-Ti3 C2 Tx /NF
electrode exhibited exceptional stability, maintaining a current OER Performance of metal oxides was improved by adding MX-
density of 100 mA cm−2 for 1200 h (Figure 7l). The stability of ene as a catalyst support, preventing catalyst aggregation and fos-
the NiFeLa-LDH/v-MXene/NF can be attributed to the higher tering strong synergy between catalyst and MXene. For example,
structural stability, as discussed in section 4.4. He and co-workers developed a bimetallic oxide alloy of Pt and
Hydrophilicity is another intriguing point about MXene that Pd on MXene to improve the OER performance in an alkaline
favors the higher interaction between active sites and water solution.[208] PtOa PdOb NPs@Ti3 C2 Tx showed a better OER ac-
molecules, as discussed in section 4.5. For example, the hy- tivity with an overpotential of 303 mV compared to other com-
drophilicity of the NiFeLa-LDH catalyst improved after adding pared catalysts. PtOa PdOb NPs@Ti3 C2 Tx showed a Tafel slope of
v-Ti3 C2 Tx , as confirmed by the contact angle measurement. The 63 mV dec−1 , significantly lower than that of pristine PtOa PdOb
contact angles were 0° in the case of MXene-included systems NPs (88 mV dec−1 ). The presence of Ti3 C2 Tx restricted the ag-
such as v-Ti3 C2 Tx /NF and NiFeLa-LDH/v-Ti3 C2 Tx /NF, indicat- glomeration of metal NPs, thus providing more catalytic centers.
ing the hydrophilicity. On the contrary, increased contact an- PtOa PdOb NPs@Ti3 C2 Tx showed good stability for 40 h at a cur-
gles were observed in systems without MXene, such as 122° rent density of 10 mA cm−2 due to the higher structural stability
and 97° for NF and NiFeLa-LDH/NF, respectively, indicating hy- of MXene. Also, in the presence of Ti3 C2 Tx support, the electronic
drophobic nature. Large exposed surface by preventing aggre- structure of Pt and Pd can be modified, which not only accelerates
gation of NiFeLa-LDH and 3D porous structure of v-Ti3 C2 Tx , the O-O bond formation but also decreases the energy barrier of
high conductivity, and hydrophilicity of MXene are the major fac- CPET in the OER process.
tors contributing to the enhanced OER performance of NiFeLa- Moreover, metal oxide NPs can assist MXene with the re-
LDH/v-Ti3 C2 Tx /NF.[173] This work also compared the OER per- stacking issue, a common problem for MXene, as discussed in
formance of NiFeLa-LDH/NF and NiFeLa-LDH/v-Ti3 C2 Tx /NF, the previous sections. For example, Fe3 O4 nanoplates success-
inferring the efficiency of MXene support. The OER performance fully alleviated the re-staking of Ti3 C2 Tx sheets, while MXene
of NiFeLa-LDH/v-Ti3 C2 Tx /NF was higher than NiFeLa-LDH/NF reduced the aggregation of Fe3 O4 , facilitating electrolyte acces-
in all the aspects, indicating a stronger synergy between NiFeLa- sibility to electrochemically active sites. Because of these rea-
LDH and v-Ti3 C2 Tx /NF than between NiFeLa-LDH and NF. sons, Fe3 O4 /Ti3 C2 Tx demonstrated the lowest overpotential of
Recently, MXene also has been assembled with layer triple hy- 290 mV at 10 mA cm−2 with a Tafel slope of 65.1 mV dec−1 among
droxides (LTHs) to enhance active sites, surface area, and conduc- the compared catalysts.[209] Similarly, metal oxide NPs benefitted
tivity. Charge transfer, surface area, and stability of LTHs have from MXene with enhanced conductivity, charge carrier concen-
been improved by preventing agglomeration and strong syn- trations, and intrinsic activity, resulting in more ionic metal cen-
ergy between MXene and LTHs after introducing MXene. For ex- ters and reduced aggregation owing to the higher SSA.[26,146,210]
ample, MXene-coupled LTH (Co4 MnFe3 /Ti3 C2 Tx ) outperformed In addition, MXene as a support shows better long-term OER
other compared catalysts toward OER activity in an alkaline stability and charge-transfer kinetics for metal oxide compared
medium. The OER catalytic activity of the Co4 MnFe3 /Ti3 C2 Tx to other 2D materials such as graphene oxide. For example, Fu
compound with an overpotential of 263 mV is the lowest com- and co-workers prepared Co-CoO heterostructure on Ti3 C2 Tx
pared to Co4 MnFe3 @GO (343 mV), Co4 MnFe3 @CNT (315 mV), to improve OER performance and stability.[148] Aggregated and
and commercial RuO2 (361 mV) at a current density of 10 mA larger particle sized (50–200 nm) pristine Co-CoO nanoplates
cm−2 . The higher performance of Co4 MnFe3 /Ti3 C2 Tx than other (Figure 8a) were uniformly distributed on Ti3 C2 Tx with an av-
2D support-based catalysts may be associated with its more ef- erage particle size of ≈25 nm (Figure 8b), which indicates the
ficient charge-transfer pathway and higher electrochemical re- strong interaction among Co-CoO and Ti3 C2 Tx . Ti3 C2 Tx effi-
action rate. Furthermore, improved stability of Co4 MnFe3 cat- ciently prevented the overgrowth and aggregation of Co-CoO
Table 1. Comparing OER performance of LDH/LTH structured electrocatalysts with and without MXene support.
Catalyst OER Overpotential [mV] at 10 mA cm−2 Tafel slope [mV dec−1 ] Cdl a) [mF cm−2 ] Refs.
Without MXene With MXene Without MXene With MXene Without MXene With MXene
FeNi-LDH 372 298 62 43 0.29 0.74 [19]

Co-LDH 390 340 98 82 – – [20]
NiFe-LDH 257 229 53 43 11.3 17.6 [147]
CoFe-LDH 352 319 66 50 25.8 36.7 [161]
NiFe-LDH – 235 80 40 0.00008 0.00026 [178]
H2 PO2 − /FeNi-LDH 270 250 53.8 46.6 5.99 6.52 [110]
Co4 MnFe3 LTH 370 263 42.4 26.3 2.43 5.59 [196]
NiFeCe-LDH 302 260 55.4 42.8 2.94 5.23 [202]
NiFeLa-LDH 249 191 67 40 11.7 15.8 [173]
NiFe-LDH 354 312 115 68 0.49 0.61 [27]
RuCo LDH – 330 – 82 – – [203]
NiCo-LDH 600 300 480 140 0.98 2.5 [204]
NiFe-LDH 336 270 101 47 1.9 16.2 [205]
(20 mA cm−2 ) (20 mA cm−2 )
Cr-FeNi-LDH 280 232 60.6 54.4 3.1 5.2 [206]
NiMn-LDH 356 294 110.5 83.7 0.102 0.426 [207]
a)
Cdl : double-layer charge capacitance. It is to be noted that Cdl values were taken at different scan rates in different works.
Figure 8. SEM images of a) aggregated Co-CoO nanoplates before anchoring on Ti3 C2 Tx and b) Co-CoO/Ti3 C2 Tx /NF with uniform dispersion of Co-CoO
nanoplates. c) Polarization curve of Co-CoO/Ti3 C2 Tx /NF in comparison with other synthesized catalysts with a scan rate of 5 mV s−1 in 1.0 M KOH. d)
Tafel and e) Nyquist plots of Co-CoO/Ti3 C2 Tx /NF and other synthesized catalysts. f) Polarization curves of Co-CoO/Ti3 C2 Tx /NF before and after 4000
cycles (the inset showing the I–t curve at a given potential to maintain 50 mA cm−2 for 72 h in 1.0 M KOH). Reproduced with permission.[148] Copyright
2021, Tsinghua university press and Springer-Verlag GmbH Germany.
Table 2. Comparing OER performance of metal oxide electrocatalysts with and without MXene support.
PtOPdONPs 320 303 88 63 – – [208]

PdONPs – 313 – 74 – – [208]
PtONPs – 343 – 86 – – [208]
RuCo2 O4 370 170 119 102 – – [28]
RuO2 – 470 – 123 – – [28]
Co3 O4 – 520 – 128 – – [28]
Fe3 O4 – 290 – 65.1 – 0.86 [209]
Co3 O4 QDs 423 340 73.24 63.97 22.2 110.2 [26]
Co3 O4 NPs 390 300 153 118 3.5 16 [146]
S-NiFe2 O4 – 270 – 46.8 – 5.11 [210]
Co-CoO 363 271 96 47 132 396 [148]
CuCo2 O4 470 380 87 71 0.37 2.1 [212]
CoNiFe2 O4 310 149 200 45 – – [213]
La0.9 Sr0.1 CoO3 406 318 97.2 88.3 3.5 6.8 [214]
Co-TiO2 – 276 – 58.3 – 6.6 [215]
a)
Cdl : double-layer charge capacitance, it is to be noted that Cdl values were taken at different scan rates in different works.
nanoplates. Co-CoO/Ti3 C2 Tx /NF demonstrated the lowest over- of 102 mV dec−1 . RuCo2 O4 /Ti3 C2 Tx /NF electrode showed a con-
potential of 271 mV at a current density of 10 mA cm−2 than stant current density of 10 mA cm−2 for more than 25 h, in-
Co-CoO/NF, Ti3 C2 Tx /NF, and RuO2 /NF in 1.0 M KOH solution dicating its long-term stability. The SMSI through strong elec-
(Figure 8c). The Tafel slope of Co-CoO/Ti3 C2 Tx /NF (47 mV dec−1 ) tronic coupling between RuCo2 O4 and Ti3 C2 Tx was assessed the-
was the lowest compared to other catalysts (Figure 8d). EIS was oretically. The DFT calculations implied that the interface be-
performed to understand the charge-transfer kinetics at the elec- tween RuCo2 O4 and Ti3 C2 Tx is pooled with charge accumula-
trode/electrolyte interface, where Co-CoO/Ti3 C2 Tx /NF showed tion, whereas the charge depletion occurred around transition
the lowest Rct of 1.9 Ω than Ti3 C2 Tx /NF (6.1 Ω) and Co-CoO/NF metal atoms in RuCo2 O4 . RuCo2 O4 region consists of positively
(9.5 Ω), as shown in Figure 8e. Also, Co-CoO/Ti3 C2 Tx /NF main- charged ions after migrating negative charges to the interface.
tained good cyclic stability in 1.0 M KOH along with long-term Then, the positively charged sites in RuCo2 O4 turn into an elec-
stability for 72 h at 50 mA cm−2 , indicating the good stability of trophilic site that easily accommodates oxygen atoms, due to
the catalyst-MXene compounds (Figure 8f). In addition, this work which more oxygen atoms can be adsorbed into RuCo2 O4 , which
compared the OER activity and stability of Co-CoO/Ti3 C2 Tx /NF is not observed in pristine binary oxides. Additionally, the desorp-
with Co-CoO/rGO/NF. In the aspects of overpotential, Tafel tion of O2 molecules would be favorable due to the reduced bind-
slope, and long-term stability, Co-CoO/Ti3 C2 Tx /NF outper- ing energy of intermediates, as confirmed by the energy shift in d-
formed Co-CoO/rGO/NF. These results suggested that the orbitals of Ru and Co toward lower energies. Electronic structure
better OER performance of Co-CoO/Ti3 C2 Tx /NF is due to tuning, optimization of adsorption/desorption properties, modi-
SMSI, high conductivity, faster charge-transfer kinetics, struc- fying electrophilicity of active sites, d-band shifting near to Fermi
tural stability, and improved surface area by preventing catalyst level were not seen in RuCo2 O4 /NF in the absence of Ti3 C2 Tx ,
aggregation. suggesting the several advantages of Ti3 C2 Tx than individual NF
Transition metal oxides with the spinel crystal structure as a support. The enhanced OER activity parameters of different
(AB2 O4 , where cation A is charged 2+ at the tetrahedral sites metal oxide-MXene catalyst compounds are listed in Table 2.
and cation B is charged 3+ at octahedra sites) are well-explored
materials for efficient OER performance.[211] Adding MXene to
spinel oxide can further enhance the OER activity of the material 5.3. Transition Metal Phosphides (TMPs) on MXene Supports
by preventing catalyst aggregation, enhancing the overall charge
transfer process, and cyclic stability of the catalyst. For exam- TMPs exhibit remarkable conductivity due to their metallic
ple, Esfandiar and co-workers reported urchin-like hierarchical nature and ample active sites resulting from their geomet-
RuCo2 O4 nanosheets attached to Ti3 C2 Tx for OER application.[28] ric structure. Usually, TMPs demonstrate significant OER ac-
RuCo2 O4 /Ti3 C2 Tx /NF demonstrated the lowest overpotential of tivity, characterized by enhanced reaction kinetics and rapid
170 mV to achieve a current density of 10 mA cm−2 in a 1.0 M charge transfer.[216–218] However, their long-term operations are
KOH solution, outperforming other catalysts in the comparison restricted due to aggregation and poor stability.[25,194,197,219] Sub-
set. RuCo2 O4 /Ti3 C2 Tx /NF also exhibited the lowest Tafel slope sequently, investigations have been performed on using MXene
Figure 9. a,b) SEM images of 3D architecture of Ti3 C2 Tx . TEM images of c) CoP@3D Ti3 C2 Tx retainment of 3D architecture of Ti3 C2 Tx after anchoring
CoP NPs and d) uniform dispersion of ultrafine CoP NPs on Ti3 C2 Tx . e) iR-corrected LSV curve of CoP@3D Ti3 C2 Tx along with other catalysts at a
scan rate of 10 mV s−1 . f) Tafel plots of different catalysts. g) Chronopotentiometric response of CoP@3D Ti3 C2 Tx and other catalysts at a current
density of 10 mA cm−2 . h) Comprehensive plots of catalytic activity and stability of CoP@3D Ti3 C2 Tx , and other catalysts, where the x-axis is 𝜂 j = 10 and
y-axis is 𝜂 j = 10 at a reaction time of 2 h. All the electrochemical experiments were carried out in O2 saturated 1.0 M KOH solution. Reproduced with
permission.[220] Copyright 2018, American Chemical Society.
as a support for TMPs to prevent agglomeration and improve overall charge transfer kinetics and conductivity through strong
the overall stability of the catalyst system. Qiu and co-workers electronic coupling. For example, Liang and co-workers syn-
prepared a CoP@3D Ti3 C2 Tx , where 3D Ti3 C2 Tx with microp- thesized a trimetallic phosphide catalyst, NiFeCoP (Ni:Fe:Co =
orous structure (Figure 9a,b) was prepared via ultrasonic-assisted 2.44:2.8:2.36) on Ti3 C2 Tx .[194] Here, Ti3 C2 Tx has been utilized
aerosol drying.[220] Here, creating 3D structure of Ti3 C2 Tx with as a conductive support that prevents the aggregation and peel-
numerous edges improved SSA and prevented the restacking of ing off of NiFeCoP NPs, while also boosting charge transfer ki-
Ti3 C2 Tx sheets. Ultrafine CoP NPs homogenously dispersed on netics owing to strong electronic coupling. The tuned electronic
Ti3 C2 Tx without aggregation and damaging 3D MXene architec- structure of NiFeCoP NPs after coupling with Ti3 C2 Tx was con-
ture (Figure 9c,d). Upon usage of 3D MXene, the SSA of the over- firmed by the DOS in the vicinity of the Fermi level, where
all catalyst drastically increased compared to pristine Ti3 C2 Tx . A NiFeCoP/Ti3 C2 Tx showed enhanced DOS compared to its pris-
highly porous and aggregation-resistant 3D Ti3 C2 Tx structure en- tine catalyst. The PDOS of Ni atoms in NiFeCoP/Ti3 C2 Tx revealed
abled higher ion transport at the electrode-electrolyte-gas triple a shift in the d-band center of Ni toward higher energies, result-
interface, while CoP assisted in reducing the reaction barrier ing from electron extraction from NiFeCoP. This facilitated op-
by exposing additional active sites during the catalytic process. timized binding strength of intermediates. The tuned electronic
CoP@3D Ti3 C2 Tx showed the lowest overpotential of 298 mV at structure of NiFeCoP/Ti3 C2 Tx contributed to improved electrical
10 mA cm−2 and Tafel slope of 59 mV dec−1 than CoP@Ti3 C2 Tx , conductivity and charge transfer kinetics, leading to a lower Rct in
CoP@3D-rGO, RuO2 , CoP, and 3D Ti3 C2 Tx (Figure 9e,f). The NiFeCoP/Ti3 C2 Tx (2.9 Ω) compared to NiFeCoP (7.3 Ω). The bet-
CoP@3D-Ti3 C2 Tx also showed around 10 h of long-term stable ter OER activity of NiFeCoP/Ti3 C2 Tx was confirmed by the lower
performance, whereas MXene-free CoP performance degraded overpotential of 240 mV at 10 mA cm−2 than NiFeCoP (270 mV)
after 4 h (Figure 9g). A plot of initial overpotential value (x-axis) and commercial RuO2 (290 mV) in 1.0 M KOH. NiFeCoP/Ti3 C2 Tx
versus overpotential value after 2 h (y-axis) shows higher stabil- also demonstrated better cyclic and long-term stability over 40 h
ity of CoP@3D Ti3 C2 Tx with a low overpotential over the time due to strong electronic coupling between NiFeCoP NPs and
compared to other catalysts (Figure 9h). Although 3D-rGO has Ti3 C2 Tx . Table 3 listed the OER parameters of transition metal
higher conductivity and SSA, CoP@3D Ti3 C2 Tx showed better phosphide supported on MXene.
OER activity and stability than CoP@3D-rGO. The reason is that
MXene-supported CoP exhibited faster charge-transfer kinetics
and structural stability due to SMSI and electronic structure 5.4. Transition Metal Chalcogenides Loaded on MXene Supports
tuning.
The effect of MXene on bimetallic/multimetallic phosphides So far, metal sulfides have been demonstrated as suitable OER
has been extensively studied, with MXene aiding in improving catalysts as they are enriched with active sites and exquisite
Table 3. Comparing OER performance of TMPs with and without MXene support.
CoP 360 298 81 51 0.33 3.51 [220]

CoP 280 230 56.5 50 5.7 11 [25]
CoP 377 280 129.5 95.4 0.36 3.49 [221]
CoP 290 260 121 51 5.38 10.39 [109]
NiFeP – 286 – 35 – 0.76 [27]
NiCoP 320 237 141 104 11 31 [197]
NiFeCoP 270 240 69 55 8.3 10 [194]
NiFeMnCoP – 244 – 41.43 – 1.5 [219]
NiFeMnCoCuP – 274 – 53.83 – 2 [219]
NiFeMnP – 294 – 41.91 – 2 [219]
Co2 P – 267 287 81 20.90 32.03 [222]
CoP-NiCoP 333 281 81.9 75.3 64.1 125.9 [223]
(50 mA cm−2 ) (50 mA cm−2 )
C,N-Co2 P 262 246 39.29 28.18 36.65 47.71 [224]
FeP-CoP 330 270 75 49 17.33 29.38 [225]
a)
intrinsic activity.[226] Nonetheless, they have not yet become vi- Additionally, metal sulfides prevent the re-stacking of MXene
able candidates for OER due to the presence of electronegative nanosheets through which a higher surface area would be pro-
S atoms that barricade metal sites and OH interactions, resulting vided during electrocatalysis. The improved surface area provides
from repulsions between S and O orbital.[227,228] To solve this is- maximum substrate area for the uniform distribution of catalyt-
sue, metal sulfides have been anchored on MXene to exploit inter- ically active metal sulfides, which exposes plentiful active sites
face engineering for better chemisorption of oxygen-containing to the electrolyte during electrocatalysis. For example, FeS2 NPs
intermediates and to make multifunctional metal sulfide elec- were introduced as a spacer between Ti3 C2 Tx sheets to prevent
trodes. Fan and co-workers prepared a porous NiCoS/Ti3 C2 Tx , their restacking. Also, Ti3 C2 Tx prevents the loss of active sites
where NiCoS NPs strongly anchored onto Ti3 C2 Tx sheets by inhibiting the aggregation of FeS2 NPs. FeS2 /Ti3 C2 Tx showed
(Figure 10a) with continuous macropores (inset of Figure 10a).[59] a lower overpotential of 240 mV than pristine FeS2 (313 mV)
The improved surface area of porous structure after preventing at 10 mA cm−2 in 1.0 M KOH solution due to the exposure of
aggregation of NPs is believed to play a major role in this study. more active sites by preventing the aggregation and restacking of
NiCoS/Ti3 C2 Tx exhibited a SSA of 55 m2 g−1 with a pore volume NPs and MXene, respectively.[229] Several factors can explain the
of 0.08 m3 g−1 , which was much higher compared to pristine improved OER activity of metal sulfides on MXene. i) Stronger
Ti3 C2 Tx (15 m2 g−1 , 0.04 m3 g−1 ) and NiCoS (8 m2 g−1 , 0.02 m3 electronegativity of MXene than metal sulfides accelerates the
g−1 ). Higher SSA and pore volume can provide a greater num- charge transfer from metal sulfide to MXene, resulting in tuning
ber of active sites on the catalyst surface and facilitate electrolyte of surface electronic structure. ii) The overall electrical conductiv-
access to the catalytic sites. NiCoS/Ti3 C2 Tx showed an overpo- ity of the catalyst compounds improves owing to the highly con-
tential of 365 mV to achieve a current density of 10 mA cm−2 , ductive MXene support. iii) Electrostatic interactions within the
which was lower than commercial RuO2 (397 mV) and other composite also shorten the electron diffusion distance. iv) MX-
compared catalysts in 1.0 M KOH solution (Figure 10b). The ene without re-stacking provides a higher surface area. v) The
NiCoS/Ti3 C2 Tx catalyst showed a Tafel slope of 58.2 mV dec−1 hierarchical structure without aggregation promotes long-term
which is the lowest compared to other compared catalysts, sug- durability by facilitating a higher exposure of active sites to the
gesting higher OER kinetics of NiCoS/Ti3 C2 Tx (Figure 10c). The electrolyte.[162,230]
catalyst also showed good durability for 6 h at a constant cur- Apart from sulfides, other chalcogenides, such as metal
rent density of 10 mA cm−2 (Figure 10d). NiCoS/Ti3 C2 Tx cata- selenides were also combined with MXene to improve the
lyst exhibited much higher double-layer capacitance (Cdl ) than overall OER activity. It is observed that SSA, charge trans-
NiCoS, NiCo-LDH/Ti3 C2 Tx , NiCo-LDH, and RuO2 (Figure 10e), fer kinetics, and OER activity of the catalyst increased after
indicating more active sites of NiCoS/Ti3 C2 Tx . Also, EIS was per- adding Ti3 C2 Tx to selenides. Yoo and co-workers reported that
formed to measure the interfacial resistance of the electrocata- Co7 Se8 @Ti3 C2 Tx exhibited an SSA of 26.7 m2 g−1 , which is
lysts. The semicircle obtained in the Nyquist plot (Figure 10f) more than double that of Co7 Se8 @ carbon fiber paper (CFP)
represents the Rct at the interface of the catalyst/electrolyte in- (11.6 m2 g−1 ).[25] The higher surface area helps in better ion
terface. NiCoS/Ti3 C2 Tx showed the smallest Rct value among all absorption which in turn increases the electrocatalytic perfor-
the catalysts, confirming favorable charge transfer kinetics. mance. In addition, the Co7 Se8 @CFP was also compared so
Figure 10. a) TEM image of a homogenous dispersion of NiCoS NPs on Ti3 C2 Tx (the inset showing continuous macropores). b) LSV curves at a scan
rate of 5 mV s−1 , c) Tafel plots, and d) chronopotentiometry curves at 10 mA cm−2 of NiCoS/Ti3 C2 Tx and other catalysts. e) Cdl of catalysts obtained
by Δj ( = Ja – jc ) plot at different scan rates. f) Nyquist plots with the bias of 𝜂 = 350 mV for NiCoS/Ti3 C2 Tx and other catalysts. All the electrochemical
experiments were carried out in 1.0 M KOH solution. Reproduced with permission.[59] Copyright 2018, American Chemical Society.
that the CFP could not prevent the aggregation of the cata- 5.5. Other Types of Catalysts Loaded on MXene Supports
lyst. Also, Co7 Se8 @CFP lacked electronic coupling and faster
charge-transfer kinetics, resulting in poor OER activity and sta- There have been limited investigations on other types of catalysts
bility. As a result, Co7 Se8 @Ti3 C2 Tx showed higher OER activ- on MXene support, such as metal nitrides, metal borides, alloy
ity with an overpotential of 291 mV at a current density of NPs, and phosphochalcogenides. This section briefly discusses
10 mA cm−2 in 1.0 M KOH solution than the Co7 Se8 @CFP the OER activity of these catalyst-MXene compounds. MXene has
of 325 mV. The Co7 Se8 @Ti3 C2 Tx also exhibited a lower Tafel been found to improve the plasmonic effect of gold NPs, which
slope of 81.5 mV dec−1 compared to Co7 Se8 @CFP (97 mV in turn increases the OER performance of Au NPs@Ti3 C2 Tx .
dec−1 ). Rct value also decreased after adding Ti3 C2 Tx to Co7 Se8 , Au NPs@Ti3 C2 Tx electrode showed a lower onset overpotential
which confirms that MXene support decreases the potential bar- (390 mV) compared to Au NPs (430 mV) and Ti3 C2 Tx (560 mV)
rier and facilitates charge transport across the selenide cata- under 525 nm laser irradiation. Au NPs@Ti3 C2 Tx exhibited a
lyst during the OER process. The post-OER analysis indicated Tafel slope of 83.3 mV dec−1 in the presence of light and 85.8 mV
a strong synergy between MXene support and selenide cata- dec−1 under dark condition, which confirms the plasmonic ef-
lyst even after prolonged OER catalysis, facilitating rapid elec- fect of the catalyst. Better OER activity of Au NPs@Ti3 C2 Tx hy-
tron transfer and improving the conductivity of the compound brid is corroborated by the synergistic effect between plasmonic
during the reaction. Also, the reconstruction of the Co7 Se8 hot electrons and Ti3 C2 Tx nanosheet. In the presence of laser
catalyst into a Co oxide/hydroxide-based catalyst during OER light, separation of hot electrons and hot holes occurs. Hot elec-
was also one of the reasons for improved OER activity in trons participate in the electrochemical reaction, whereas hot
Co7 Se8 @Ti3 C2 Tx , where oxyhydroxides serve as the electrochem- holes on the Au NP surface trap the electrons, which facilities
ically active sites. Similarly, better OER performances were found the formation of Ti3+ and Ti4+ species with higher catalytic ac-
in 1T/2H MoSe2 /Ti3 C2 Tx and Ni-MoSe2 /Ti2 NTx . Here, the im- tivity. This overall process significantly enhanced the OER of Au
proved OER performances were attributed to the highly con- NPs@Ti3 C2 Tx , which is absent in the case of only Au NPs.[236]
ductive MXene providing faster charge transfer kinetics and Recently metal nitrides have been explored as electrocatalysts
abundant active sites of MoSe2 . In addition, the formation of due to their high electrical conductivity and noble-metal-like
Ti─O─Mo covalent bond between MoSe2 and MXene improved properties. However, their sluggish kinetics in an alkaline
the stability and catalytic activity of these compounds.[220,221] medium restricts their performance.[203] Combining metal
Table 4 listed different OER parameters of chalcogenides/MXene nitride with MXene can optimize the electronic structure, im-
compounds. proving the intermediate adsorption/desorption properties and
Table 4. Comparing OER performance of transition metal chalcogenides electrocatalysts with and without MXene support.
FeS2 313 240 64 58.7 1.14 2.58 [229]

CoS2 323 270 96 92 9 28 [162]
CoS – 310 – 40.2 – – [230]
NiCoS – 365 73.7 58.2 1.2 2.4 [59]
Ni3 S2 – 410 – 173 – 16.4 [233]
Ga-Ni3 S2 – 340 – 112 – 21.1 [233]
Co7 Se8 325 291 97 81.5 1.4 2.5 [25]
1T/2H MoSe2 397 340 111 90 3.7 21.8 [220]
MoSe2 541 328 144 96.4 7.5 26.4 [231]
Ni-MoSe2 – 270 – 81.1 – 75.4 [232]
NiFeS 300 276 210 177 – – [234]
(20 mA cm−2 ) (20 mA cm−2 )
Co3 S4 -Ni3 S2 – 186 – 97 – 8.95 [235]
a)
enhancing the water electrolysis performance. Yan and Zhang Cr2 CO2 MXene as OER catalysts.[240] They explored various
prepared RuCoN/Ti3 C2 Tx heterostructure and applied it as SACs with transition-metal atoms (TM: Mn, Fe, Co, Ni, Mo,
an OER catalyst, which showed an overpotential of 238 mV Ru, Pd, Ag, Ir, and Au) on Cr2 CO2 MXene for OER, calculating
to achieve a current density of 10 mA cm−2 and maintained the theoretical onset overpotential by evaluating the free ener-
stable performance for 20 h.[203] The excellent OER activity gies of the four fundamental reactions involved in OER. Their
of Ru-CoN/Ti3 C2 Tx was attributed to accelerated adsorp- findings indicated that pristine Cr2 CO2 was not OER-active and
tion/desorption of intermediates facilitated by the tuned unsuitable as an OER catalyst. Among the investigated SACs,
electronic structure of RuCoN after coupling with Ti3 C2 Tx . Ni/Cr2 CO2 exhibited the lowest OER overpotential of 230 mV.
Furthermore, a highly resilient interfacial junction between Ru- Binding energy and charge transfer calculations revealed the
CoN and Ti3 C2 Tx accords beneficial mass and charge transport, stronger coupling between Cr2 CO2 and Ni. Furthermore, ab-
robust morphology, and higher structure stability, contributing initio molecular dynamics simulations and climbing nudged
to remarkable OER activity. Furthermore, the addition of MXene elastic band calculations confirmed that adding Cr2 CO2 as a
addressed the issue of poor electron transport between metal support prevented the aggregation of SACs. The absence of
borate/boride and electrolyte during the electrocatalytic process. Ni3 and Ni4 cluster formation demonstrated the stable binding
For example, the introduction of Ti3 C2 Tx resulted in boosted of Ni atoms on the surface of Cr2 CO2 . Similarly, a series of
charge transfer in the hybrid catalyst, which restricted the SACs comprising various transition-metal elements (Ti, V, Cr,
agglomeration of CoB.[237] Mn, Fe, Co, Ni, Cu, Zn) anchored on M2 NO2 MXenes (M =
Phosphochalcogenides or thiophosphite materials (MPSx ) Ti, V, Cr) were investigated for their OER activity. The results
have gained new interest due to their high catalytic activities, indicated that Cu/Ti2 NO2 exhibited the best OER electrocatalytic
which stem from the enriched electronic structure of metal cen- performance among all combinations, with an overpotential
ters by the existence of both sulfur and phosphorous.[238,239] Yan of 0.24 V for the four reaction steps. The study also suggested
and co-workers investigated the synergy between MXene and that Cu/Cr2 NO2 could be a potential candidate for an OER
MPS3 to improve catalytic activity by tuning the surface electronic catalyst, with an overpotential of 0.28 V. Table 5 listed the OER
structure.[62] They prepared a Ni0.7 Fe0.3 PS3 @Ti3 C2 Tx electrocat- parameters of all other catalysts supported on MXene.
alyst that exhibited a lower overpotential of 282 mV compared
to Ni0.7 Fe0.3 PS3 (292 mV) at 10 mA cm−2 in 1.0 M KOH. MX- 6. Summary and Future Perspectives
ene provided higher structural stability to the MPS3 catalysts, as
confirmed by TEM and HRTEM characterization before and af- In this review, 2D MXene was introduced as a promising candi-
ter 10 and 15 h of OER. The thin amorphous layer surrounding date for support materials toward OER due to its unique prop-
the crystal phase remained intact even after prolonged OER, in- erties, including SMSI, good hydrophilicity, large surface area,
dicating the structural stability of Ni0.7 Fe0.3 PS3 @Ti3 C2 Tx catalyst high electrical conductivity, and long-term durability. From the
compound. perspective of utilizing MXene not only as a support but also as a
In addition to experimental studies, there have been limited catalyst-support hybrid, an extended OER mechanism based on
theoretical investigations on the oxygen evolution reaction (OER) the formation of M-OOH intermediates was described. Further-
activity of MXene supports, particularly focusing on Cr-based more, efficient synthetic strategies such as wet-chemical, phase-
MXenes. For instance, Zhang and co-workers conducted a transformation, and electrodeposition techniques for the suc-
theoretical study on single-atom catalysts (SACs) anchored on cessful preparation of MXene and catalyst-MXene compounds
Table 5. Comparing OER performance of catalyst-MXene compounds.
FeNi 282 195 44.18 42.78 – – [241]

Ni0.7 Fe0.3 PS3 292 282 43.4 36.5 0.605 0.755 [62]
CoN 402 365 127 112 4.0 7.5 [203]
Ru-CoN – 238 – 80.2 – 15.2 [203]
CoB 310 250 73 53 – – [237]
CoBDC – 410 48.8 48.2 1.0 9.6 [160]
FeOOH QDs 490 420 52.2 31.7 0.048 0.43 [242]
FeOOH 470 400 107 95 0.34 1.46 [243]
P-MoO3 -FeCo LDH 211 179 – 40.44 – 9.0 [244]
RuCo 313 253 66.7 61.3 16.77 35.01 [245]
Co3 O4 @g-C3 N4 387 247 187.36 144.7 0.795 1.69 [246]
Co@V2 CTx – 242 – 90.4 – 113.5 [247]
Co@Nb2 CTx – 310 – 100.2 – 98.8 [247]
Co@Ti3 CTx – 388 – 109.2 – 91.1 [247]
Ag 560 310 127 114 – – [248]
NiFe-LDH-CoP2 -MnP 259 200 72.95 17.72 1.7 3.71 [249]
NiCo – 220 – 94 – – [250]
a)
were summarized. In particular, the crucial properties of MXene origins of hydrophilicity mechanism in MXene require further
as the support material benefiting improved OER performances investigations.
were discussed in detail in this review. In this regard, examples In terms of catalyst-MXene compounds, defect engineering of-
of catalyst-MXene compounds, such as LDH, metal oxide, TMP, fers a promising approach to improve OER activity. Defect gener-
chalcogenide, and other materials, with their significantly im- ation in both catalyst and MXene support could be a challenging
proved OER performances were presented. yet intriguing task for improving electrocatalytic activities. Fur-
Although MXene has been successfully utilized as a sup- ther, the well-controlled surface morphology of MXene can be ap-
port material for OER catalysts, several challenges have to be plied to catalyst-MXene compound synthesis to improve electro-
addressed, ranging from fundamental understanding to prac- chemical properties. Coupling of F-free MXene with the catalyst
tical utilization. In terms of MXene synthesis, the preparation is still an area that needs to be explored for improved electro-
method for MXene with respect to OER activity remains am- chemical activities and stability. Most importantly, many studies
biguous. While literature suggests that F-terminated MXene has have utilized Ti3 C2 Tx as a support. Therefore, we propose that
lower OER activity and stability, most studies have utilized F- there is a good opportunity to use a different “M” instead of Ti
terminated MXene as a catalyst support. Surface and structural for the M2 XTx and M4 X3 Tx structures to modify SMSI. Further-
modifications can be a realistic way to improve the conductivity more, large-scale synthesis and commercialization of catalyst-
and SSA of the F-terminated MXene. To this end, constructing MXene compounds with uniform particle distribution, higher
an accurate structure of the modified Mn+1 Xn Tx based on the un- surface area, improved SMSI, and better OER performances still
derstanding of the structural changes of MXene concerning the T remain important tasks. Due to the various favorable properties
and x is of utmost importance. Simultaneously, investigation of of MXene, the OER performance of catalysts has been success-
the electronic, thermal, magnetic, optical, mechanical, and cat- fully enhanced. Therefore, it is crucial to acquire a comprehen-
alytic properties of the modified MXene should be followed. Fu- sive understanding of the fundamental principles governing the
ture studies may explore F-free MXene to improve OER activity interaction between MXene and catalyst particles to elucidate the
and stability. Obtaining new types of MXene with high efficiency bond strength and promote fast electron transfer of reactants. De-
could involve the addition of multiple transition elements, and si- spite the remarkable stability exhibited by the MXene supports
multaneous addition of C and N at the x position, which is one of under severe catalytic conditions, uncertainties persist regarding
the most challenging topics in modifying MAX phases. In addi- their stability in aqueous environments. Therefore, comprehen-
tion, easier and safer methods must be adopted instead of highly sive and meticulous exploration is essential to unveil the funda-
toxic HF etching. Later, large-scale synthesis and commercializa- mental mechanism that contributes to the high stability observed
tion of MXene should focus on improving quality, porosity, and in the MXene-catalyst composites.
achieving a monolithic shape. Furthermore, the evolution of hy- In terms of the OER mechanism, a profound understand-
drophilicity in MXene is still in its infancy, and the fundamental ing of the OER mechanism of MXene coupled catalysts requires
thorough investigation, especially the LOM of OER has been least Keywords
investigated. Understanding the LOM associated with oxygen va-
cancies creation and increasing vacancy concentrations poses a 2D materials, MXenes, support materials, oxygen evolution reaction, water
electrolysis
challenging task. OER activity can be further improved by ac-
tivating lattice oxygen, which can be adapted to catalyst-MXene
Received: May 31, 2023
compounds. The role of MXene in elucidating OER mechanisms Revised: July 20, 2023
is lacking in the current literature, where most studies only fo- Published online:
cused on the catalysts. Thus, further investigations are required
to comprehend the relationship between OER activity and LOM
of catalyst-MXene compounds.
Simultaneously, state-of-the-art ex-/in-situ measurements to
analyze the physicochemical and electrocatalytic properties of [1] S. Chandrasekaran, D. Ma, Y. Ge, L. Deng, C. Bowen, J. Rosco-w, Y.
catalyst-MXene compounds would be highly beneficial in provid- Zhang, Z. Lin, R. D. K. Misra, J. Li, P. Zhang, H. Zhang, Nano Energy
2020, 77, 105080.
ing deeper insights into the effect of MXene, thus, speeding up
[2] Y. Luo, Z. Zhang, M. Chhowalla, B. Liu, Adv. Mater. 2022, 34,
the commercialization of catalysts. For example, structural evo- 2108133.
lution and degradation of MXene during OER could be analyzed [3] M. A. Khan, H. Zhao, W. Zou, Z. Chen, W. Cao, J. Fang, J. Xu, L.
by performing pre- and post-OER using ex-/in-situ methods. Zhang, J. Zhang, Electrochem. Energy Rev. 2018, 1, 483.
Although recently reported catalyst-MXene compounds demon- [4] B. Ruqia, S. Choi, ChemSusChem 2018, 11, 2643.
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Bhargavi R Anne received her Ph.D. degree in Materials Process Engineering from Kyushu University,
Japan (MEXT Scholar, 2020). After her postdoctoral research in the Choi group at Kyungpook National
University, Korea, she joined the National Institute of Technology Warangal, India as an Assistant
Professor (ad-hoc). Her research interests include correlating defects to material properties at micro
and nano-level.
Joyjit Kundu is currently a postdoctoral researcher at Kyungpook National University under the super-
vision of Prof. Sang-Il Choi. He received his Ph.D. degree in materials science from Indian Institute of
Technology Kharagpur, India (2021). His research interests include electrochemical water splitting,
CO/CO2 reduction, and anion-exchange-membrane-water-electrolyzer.
Sang-Il Choi received his Ph.D. degree in inorganic chemistry from the KAIST (2011). After his post-
doctoral research in the Xia group at the Georgia Institute of Technology, USA, he joined the Kyung-
pook National University in 2015 as an associate professor. He is the recipient of the 2018 POSCO
TJ Park Science Fellowship and the 2023 Prime Minister’s Citation of Korea. His research interests
include the design and synthesis of nanomaterials and exploration of their applications in electro-
catalysis.

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REVIEW

A Review on MXene as Promising Support Materials for

Therefore, developing catalyst supports

catalysts can be controllable by adding or removing MXene. For 5. OER Performances

FeNi-LDH 372 298 62 43 0.29 0.74 [19]

PtOPdONPs 320 303 88 63 – – [208]

CoP 360 298 81 51 0.33 3.51 [220]

FeS2 313 240 64 58.7 1.14 2.58 [229]

Table 5. Comparing OER performance of catalyst-MXene compounds.

FeNi 282 195 44.18 42.78 – – [241]

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