1 s2.0 S2352152X22017534 Main

Journal of Energy Storage 55 (2022) 105765
Contents lists available at ScienceDirect
Journal of Energy Storage

journal homepage: www.elsevier.com/locate/est
Review Article
MXene based hybrid materials for supercapacitors: Recent developments

and future perspectives
Susmi Anna Thomas a, 1, Abhinandan Patra b, 1, Badria M. Al-Shehri c, d, e, Manickam Selvaraj c, d,
Arun Aravind a, *, Chandra Sekhar Rout b, *
a
Centre for Advanced Functional Materials (CAFM), Postgraduate and Research Department of Physics (Affiliated to University of Kerala), Bishop Moore College,
Mavelikara, Alappuzha, Kerala 690110, India
b
Centre for Nano and Material Sciences, Jain University, Jain Global Campus, Jakkasandra, Ramanagaram, Bangalore 562112, India
c
Department of Chemistry, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi Arabia
d
Research Center for Advanced Materials Science (RCAMS), King Khalid University, P.O. Box 9004, Abha 61413, Saudi Arabia
e
Unit of Bee Research and Honey Production, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi Arabia
A R T I C L E I N F O A B S T R A C T
Keywords: With respect to the advancement in electronics and other related technologies, in this current era of industrial
2D materials revolution there exists a higher demand for efficient energy storage devices which possess properties such as low
MXenes cost, flexibility, longer life, etc. 2D layered materials have received significant attention in the current century
Heterostructure
due to its physical, mechanical and optical properties that are suitable for the fabrication of high-performance
Supercapacitors
energy storage devices. Among various 2D materials, transition metal nitrides/carbides collectively known as
TMDCs
Metal nitrides/carbides MXenes got profound interest in material science owing to its smaller thickness, bandgap tunability, good
conductivity, better mechanical properties, hydrophilicity, availability of abundant active edge sites and tunable
electrochemical properties, etc. Due to these advantages, MXene based materials are demonstrated to be act as a
suitable electrode for high performance energy storage devices especially in supercapacitors. But, MXenes have
some demerits due to the aggregation and restacking of its layers which stand as a hurdle for its further
exploration. Herein, in the present audit, an in-depth study on the supercapacitor applications of MXenes and its
hybrids with carbonaceous materials, conducting polymers, transition metal dichalcogenides (TMDs), transition
metal oxides (TMOs), etc., is deliberated thoroughly and the fundamental properties, synthesis tactics and
etching procedures comprising various kind of MXenes is also highlighted. Likewise, we primarily focus on the
current developments, challenges and the future perspectives of MXenes based hybrid materials for super
capacitor applications. This review not only includes the pioneering studies but also comprises of very recent
intriguing ones along with the research gap which is conversed through the future perspective discussions.
1. Introduction based on electrochemical reactions, known as supercapacitors/electro

chemical capacitors are being explored extensively [3]. The researchers
Energy storage applications are highly discussed in the present have been investigating the supercapacitors (SCs) based on different
context due to the rapid depletion of fossil fuels and tremendous in emerging materials in detail, in order to avoid the constraints associated
crease in human population. Different types of batteries such as sodium with the battery type electrode material. However, low energy density of
and lithium-ion batteries [1] and capacitors are vastly praised among all electrochemical capacitors is one of the main challenges which can’t be
these electrochemical energy storage systems [2,3]. But the low cycle overlooked. The low energy density is mainly by the carbon-based
life, shorter life time and limitations in power density of the available supercapacitors in which electrochemical double layer formation in
energy storage devices introduced a demerit for its further exploration. the electrode-electrolyte interface takes place (often referred as elec
In order to avoid these issues, the next generation energy storage devices trostatic double layer charge storage mechanism (EDLC). Thus, other
* Corresponding authors.
E-mail addresses: arun@bishopmoorecollege.org (A. Aravind), r.chandrasekhar@jainuniversity.ac.in (C.S. Rout).
1
Authors contributed equally.
https://doi.org/10.1016/j.est.2022.105765
Received 7 July 2022; Received in revised form 29 August 2022; Accepted 23 September 2022
Available online 7 October 2022
2352-152X/© 2022 Published by Elsevier Ltd.
S.A. Thomas et al. Journal of Energy Storage 55 (2022) 105765
type of supercapacitors based on faradic charge storage mechanisms developments on the supercapacitor applications of MXene and its hy
(pseudocapacitive mechanism) are being explored which possess higher brids with carbonaceous materials, conducting polymers, transition
energy density than the EDLC supercapacitors. But still both these type metal dichalcogenides (TMDs), transition metal oxides (TMOs), etc. is
of electrode materials have their own drawbacks in achieving high being furnished. The research gap comprising of MXene based electrodes
performance energy storage devices [4,5]. In this regard, huge research for device application and regarding its need in global energy market,
activities are being carried out in recent years to improve the perfor various strategies for enhancing the electrochemical properties and the
mance of the supercapacitor by applying different novel emerging cost optimization has also been elucidated through the future perspec
advanced materials as the electrodes [2–7]. tives. Fig. 1 displays the schematic illustration on the content of the
From the beginning of 20th century, graphene is being considered as review.
an important pioneer of two-dimensional layered material for different
applications due to its high transparency, high thermal conductivity, 2. Crystal structure, synthesis and properties of MXenes
excellent opto-electronic properties, high Young’s modulus and high
specific surface area [8]. The electrode materials with graphene and 2.1. Crystal structure
CNT electrodes have large surface area and good mechanical stability
[9]. In 2D materials based EDLC supercapacitors, the improved charge MXene is prepared by the removal of element A from parent MAX
storage mechanism is controlled by the higher surface area of electrodes, phase with formula Mn+1Xn (n = 1, 2, 3). MAX phases have a layered
but in the case of pseudocapacitors, charge storage is obtained by the ion hexagonal structure with P63/mmc symmetry, where M layers are
intercalation in aqueous solution where the ions intercalate into the nearly closely packed and X atoms fill octahedral sites [22]. Due to this,
layers reversibly and occupies to the electrochemically active surfaces Mn+1Xn layers are interleaved with the A element, which is metallically
on the layers contributing to the improved energy storage mechanism. bonded to the M element. A strong covalent/ionic/metallic character is
To enhance the energy density of SCs, TMOs such as ruthenium dioxide exhibited by M–X bond and a metallic M–A bond exists there. In the
(RuO2) [10], manganese dioxide (MnO2) [11], conducting polymers case of MAX phase, the bonds are too strong and there exists a slightly
such as polyaniline (PANI) [12], polypyrroline (PPy) [13], transition weaker M–A bond in comparison to M–X bonds with properties of
metal dichalcogenides (TMDs) [14], transition metal trichalcogenides relative bond energies. MXene have Mn+1XnTx formula with Tx repre
(TMTCs) [15], etc., are being used as the electrodes in order to achieve sents –O, –OH, –F surface terminated functional groups attached over
large power density. But the lower electrical conductivity in metal ox M atoms after etching. Generally, MXenes shows three formulas: M2X,
ides and hydroxides are hindering its cyclic performance and power M3X2 and M4X3 where M is the early transition metal and X is carbon(C)
density [16]. Also, 2D TMDs based electrodes lead to agglomeration due and nitrogen (N). For M2X, the formation of a honeycomb lattice takes
to its large surface energy and it possess higher resistance when utilized place. There are more than 100 types of MXenes are discovered by ab-
as an electrode material and prevents their use for the large-scale elec initio calculations and greater than 25 types of MXenes are obtained
trochemical energy storage device fabrication [17]. In this context, to by experimentally till now. This functional group terminated MXenes
solve the difficulties with these materials, another new class of material show three configurations as shown in Fig. 2. For Type 1, on the top of
is come into picture; MXenes are being explored as electrode materials hollow site of three neighboring X atoms, functional groups are located,
owing to its better structural properties and high active sites for the which are pointing to the M atoms in second Ti atomic layer. In Type 2,
faster charge transfer processes and redox reactions [17]. on top of topmost sides of X atoms functional groups are located. For
Generally, group IV-VI transition metal carbides and nitrides are Type 3, it produces a combined structure of Type 1 and Type 2, where
discovered in 20th century and the application of these materials for one of the functional groups is located on the top of hollow sites of X
energy storage fields are explored after the discovery of their catalytic atoms in one side and another functional group is located on above the
properties in 1970s [18]. One of the break-through explorations top site X atom on the other side where the Type 1 is more stable
happened in 2011, with the discovery of first MXene Ti3C2Tx by Yury [24–28]. With respect to terminations, the relative position of MX layers
Gogotsi and team [19]. More than 25 different compositions of MXenes forms a two-stacking type arrangement; one is a simple hexagonal and
have been synthesized and studied later. There are several other MXenes other is bernal stacks which are connected through the dihydrogen
such as Ti2CTx, Nb2CTx, Mo4VC4Tx, Mo2ScCTx, etc., are also introduced bonding between surface groups. The interlayer atoms are joined by
later on. Transition metal carbides and nitrides have the general formula strong covalent and ionic bonds [23,25,27]. Recently, there are various
Mn+1XnTn, where M is a transition metal, X is the carbon and/or nitrogen studies are established for the case of a solid solution of various transi
̍̍ ̍
and T represents –OH, –F, –O, etc., like surface termination groups. tion metals such as M̍ and M̍ ̍ and with A element as A ̍ and A in
Conductive nature and charge transfer properties due to the variable combination of X species like C or N introducing the generation of MAX
oxidation number holding transition metal M along with the stacked phase alloy and the synthesis of corresponding MXene. With respect to
structure of MXenes make them better candidate for electrochemical this, there are some alloys based MXenes such as (Ti0.5Nb0.5)2C,
applications especially for energy storage devices [18–22]. However, (V0.5Cr0.5)3C2, Ti3CN, etc., are experimentally synthesized. With respect
MXenes consist of surface terminal functional groups and possess to the proper selection and stoichiometry of M̍ and M̍ ̍ , A and X, we can
metallic conductivity with faster redox reactions and higher charge- synthesize two different phases of MAX phase with ordered arrangement
storage characteristics [23,24] in comparison with other 2D materials, of double transition metals known as, oMAX and iMAX phases. MAX
especially due to its tunability in electrical and magnetic properties. The phase possessing an out-of-plane ordered double transition metals, like
presence of excess number of terminal groups such as oxygen and M2̍ M̍ ̍ AX2 and M2̍ M̍ ̍ AX3 forms the oMAX phase. As like as the tradi
fluorine contained in MXene sheets collapse the layered structure by tional MAX phase, the transition metal layers on oMAX phase is occu
heaping of these layers from the lamellar structure. But restacking and pying with only one type of M or M̍ which sustain the similar
aggregation stand as the major problem for the further exploration of 2D crystallographic space group symmetry as P63/mmc. Mo2TiAlCl2,
layered materials especially in the case of MXenes. Thus, various at Mo2Ti2AlCl3, Mo2ScAlCl2 and Cr2AlTiCl2 are the examples of oMAX
tempts are established to overcome the problems regarding MXenes as phases which were synthesized so far. In the case of iMAX phase, the
an electrode, thereby the idea of hybrid/heterostructure with other MAX phases are possessing an in-plane orientation and it hold the for
materials such as carbon species, TMDs, conducting polymers, TMOs, mula as (M2/3̍ M1/3̍ ̍ )2AX. Apart from conventional MAX and oMAX
etc., are developed [23]. Herein, the present review provides the brief phases, the layers of iMAX phases are contains both M̍ and M̍ ̍ . Besides
information about the properties of MXenes and the influencing factors the hexagonal arrangement in conventional MAX phases, in the case of
which play a major role in the charge storage performance of super iMAX phases the atoms are generating a Kagome-like lattice. This is due
capacitors. Additionally, a detailed discussion about the recent to the variation in atomic size, where M̍ <M̍ ̍ , thereby A atoms producing
2
Fig. 1. Brief outline of the content of the review.
a deviation from the hexagonal arrangement and creating a Kagome-like Fig. 4.

lattice and it possess a space group symmetry as C2/c. iMAX phases such MXene etched by the pure HF solution possess an accordion-like
as (M2/3̍ M 1/3̍ ̍ )2AlC where M̍ = W, Mo, Cr and M̍ = Sc, Y and (M2/3̍ Zr1/3̍ morphology in which the van der Waals bonds and hydrogen bonds
)2AlC where M̍ = Cr, V are synthesized till now [27,28]. bind the 2D layers. If diluted HF is used, the MXenes morphology is
̍
changed to thicker multilayer lamellas with lower interlayer gap
2.2. Synthesis methods of MXenes [23,27]. By using a low concentration HF for etching, MXene in
tercalates large H2O molecules with higher mobility to the interlayer
There are different methods for the synthesis of MXenes which are and consists of large open interlayer spaces to facilitate wide range of ion
basically two types: firstly, the top-down method in which the conver accessibility towards the active sites and increases the capacitance. For
sion of MAX phase towards MXene takes place and in the bottom-up the diffusion of ions towards electrochemically active sites to the
approach, the reaction of individual precursor materials lead to the inetrlayers of MXene which need large active energies, so we need
formation of MXene. For the top-down method, a 2D structure is ob mechanical exfoliation such as scotch tape exfoliation and higher power
tained from its 3D bulk state by weakening the interlayer bonds in bulk. sonication for the preparation of multilayer HF etched MXene. The
Exfoliation is a common top-down method but this method is not scotch tape exfoliated MXene consists of higher quality with a smaller
applicable to every MXenes due to the existence of the strong bonds number of defects. Simple mechanical exfoliation produces a smaller
between M and A layers. Thus, some other methods are developed for amount of single layer due to strong interlayer interaction which is
the preparation of MXenes from its bulk counterparts; basically, these about two-fold to six-fold stronger when compared with MoS2 and
methods involve different etching processes [22,23]. Different synthesis graphite. Higher power ultrasonication possesses greater efficiency than
methods of MXenes are summarized in Fig. 3. scotch tape exfoliation. Multilayered MXene by chemical intercalation
delamination is a suitable choice. It is possible to intercalate the
2.2.1. HF etching multilayered MXene by various organic molecules like N, N-dimethyl
HF etching is a wet chemical method where the species MXenes are sulfoxide (DMSO)/hydrazine, urea and N, N-dimethylformamide in
formed by the selective etching of reactive A layers. MAX phase is a order to reduce the interlayer coupling. Intercalation with liquids such
combination of layered ternary nitrides and carbides. Chemically active as DMSO, 1-PrA and TBAOH between MXene with mild sonication in
A-atom layers are weakly bound to the MAX phase thus producing the water produce a delamination towards separate sheet where DMSO is
selective etching of ‘A’ element layers. Usually, aqueous hydrofluoric only applied for Ti3C2Tx MXene and others are applicable for all
acid (HF) solution is used to etch the MAX phase to produce MXenes. By MXenes. Liquid based delamination need long time and intercalation of
the removal of ‘A’ element layers the balancing MX layers are rapidly Na+, K+, NH+, etc., like inorganic cations can able to do it electro
terminated by –O, –F, –OH or –H surface groups with M n+1XnTx chemically. Ti3C2 can also be able to synthesize by using various pre
formula [23]. Pictorial representation of HF etching process is given as cursors such as Al etching from Ti3AlC2 in fluorine and solution with
3
Fig. 2. Geometries of Ti3C2 monolayer with hydroxylated and fluorinated forms as (a) side view of the bare Ti3C2 monolayer composed of a quintuple layer with Ti
(1)–C–Ti(2)–C–Ti(1) stacking modes (left) and the computed spin density distribution (middle); side views of (b) I-Ti3C2F2, (c) IITi3C2F2, (d) III-Ti3C2F2, (e) I-
Ti3C2(OH)2, (f) II-Ti3C2(OH)2, and (g) III-Ti3C2(OH)2; (h and i) the top views of I-Ti3C2F2 and IITi3C2F2, in which the F groups are located above the hollow sites
between the three neighboring C atoms and above the topmost C atoms, respectively. III-Ti3C2F2 is a combination of I-Ti3C2F2 and IITi3C2F2, in which the F groups
are located at the hollow sites on one side and at the C atoms on the other side. The geometrical arrangements of OH groups for I-Ti3C2(OH)2, II-Ti3C2(OH)2, and III-
Ti3C2(OH)2 are structurally similar to their fluorinated analogue Reprinted with permission from [27] Copyright (2012). American Chemical Society.
acid or with oxidant assisted etching on Si from Ti3SiC2 [27–32]. by using these etchants consist of similar type accordion-like
morphology [23,34,35]. With this etching process NH+, Na+, K+ and
2.2.2. Acid/fluoride salt (hydrofluoride etching) Fe3+ is intercalated to the MXene layers rapidly. This cation intercala
For HF etching fluorine containing salts like (NH4) HF2, HCl/NH4F tion introduces an open and homogeneous layer structure than pure
and HCl/FeF3, etc., are also used as the alternative milder etchants for MXene. In the etching of Ti3AlC2 with HCl/FeFe3 there exists a partial
the in-situ production of MXenes [33]. All these etchants are applied for oxidation of Ti surface by Fe3+ cations due to the Al extraction. Among
the preparation of Ti3C2Tx MXene, but it does not assure the preparation this acid/fluoride salt, HCl/LiF is an effective etchant. With the suitable
of other MXenes. V2C MXene is prepared by the NaF/HCl etchant. concentration of LiF and HCl, intercalation of solvated Li+ ions produce
Hydrofluoride assisted etching takes longer time than pure HF etching, delamination. So that MXene flakes consist of single or few layers with
but it provides a credit for safety in operations. But the prepared MXenes less defects are able to synthesize by just shaking without the aid of
4
Fig. 3. Top-down and bottom-up methods for the synthesis MXenes.
Fig. 4. Pictorial representation of etching processes of MXene from MAX phase.
sonication or intercalation (Fig. 5). Thus, it is possible to keep the grain by the selective etching of Si layers with the mixture of HF and oxidants
size and shape of flakes matching to select a correct MAX phase for contain etchants like HF-FeCl3, HF-H2O2, HF-HNO3, etc. They found that
developing MXenes. This hydrofluoride etching provides large number the etching process depends upon the concentration of HF, etching time
of advantages for MXene synthesis other than its demerit with long and temperature. Because of its low cost and easy way of operation,
etching time [36–39]. Alhabeb et al. [36] prepared MXene from Ti3SiC2 carbides and carbonitrides are easily synthesized by this route but
5
Fig. 5. (a) Schematic representation of MXene with different flake size, (b) light scattering analysis of MXenes with red arrow gives the wide distribution of particle
sizes in synthesized MXenes without centrifugation (c) representing the variation of influence of sonication power and time (d) indicating the polydisperse MXene
flakes possible to separate by sucrose in 20–66 w/v%. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)
Reproduced with permission from [29]. Copyright (2018) American Chemical Society.
nitrides are difficult. Etching process with HF etchant results in the HF, basically due to its toxic nature and the existence of unfavorable –F
introduction of –F surface terminal groups which reduce the perfor groups for supercapacitor performance of MXene, thus, new methods
mance of electrode devices and its operation is producing a negative with fluorine free routes are developed [40]. Xuan et al. [41] reported
impact to the environment. It is possible to replace the –F functional that, it is possible to remove Al layer from Ti3AlC2 by tetra methyl
groups in the MXene by –OH groups by the treatment with aqueous ammonium hydroxide (TMAOH) when performing a pre-treatment with
solution where the Ti–F bond weakens at high pH. In comparison with 20-30 wt% HF for MAX phase in short duration. But reproducibility with
HF etching, by using etching agents like HCl/LiF, NH4HF2 produce rapid the application of TMAOH is less, thus their work reveals that HF and
etching and results the intercalation of Li+, NH4+ and intercalation of TMAOH is collectively producing a contribution for etching Al from
water between layers introduces the interlayer spacing thereby Ti3AlC2.Thus, inorganic alkalis are highly used for etching MXene from
improving the electrochemical performance of energy storage. Thus, MAX phase other than organic alkalis. By considering the features of
some modifications are needed for the HF etching methods. He et al. alkali based etching procedure, T.Li et al. [42] prepared Ti3C2Tx MXene
[30] prepared V2CTx MXene by NaF + HCl as etchant at 90 ◦ C for 72 h with a purity of 92 wt% in alkali assisted hydrothermal method. Here
there exist a selective etching of Al layers from V2AlC MAX phase. The they treated the parent Ti3AlC2 MAX phase in NaOH water solution in
prepared electrode material delivers a specific capacitance of 317.8 F/ hydrothermal treatment with the application of argon atmosphere for
cm3 with 89.1 % of capacitance retention after 5000 cycles in sea water avoiding the oxidation. By the various thermodynamic reactions in
electrolyte. assistance of Bayer process (according to Bayer process higher temper
ature and high alkali concentration is supports for dissolving the Al
2.2.3. Alkali etching oxide/hydroxides, thereby a removal of Al phases) there exists a trans
For MXene preparation using acidic solution, etching protons and formation of parent MAX phase to the fluorine free MXene and a sche
fluoride ions is important. By considering the difficulties associated with matic diagram of synthesis procedure followed by them is given as
6
Fig. 7. Alkali etching process have some advantages which provide 2.2.6. Bottom-up methods
improved interlayer spacing and reduced –F terminations, beyond this Basically, the bottom-up method involves chemical vapor deposition
MXene flakes is needed to be delaminate further for its synthesis (CVD) and atomic layer deposition (ALD). The bottom-up method fa
[42,43]. cilitates crystal perfection and makes them as robust and stable. This
feature in tunability of layer number with transition metal carbides
2.2.4. Molten salt etching produces the 2D crystals whose properties match with bulk carbides
In order to avoid the difficulties occurred with HF based etching, [46]. Xu and co-workers [47] prepared α-Mo2C structure by CVD from
material scientists are put forward an approach where they used molten methane over a bi layer copper foil substrate standing on molybdenum
salts for etching MXene from MAX phase. In Lewis acid molts, A-site foil. CVD method is a feasible method for fabricating monolayer carbides
etching of MAX phase is verified by the preparation of different MXenes and other transition metal nitrides. MXenes synthesized through CVD
with Si, Zn and Ga as A site element of MAX phase [44]. This method is method possesses larger crystallinity than the etched MXenes. MXenes
basically used for the synthesis of nitride MXenes because of its higher heterostructures and various stoichiometries can be prepared by this
energy of formation as like as carbide MXenes. The reduced cohesive method. Similarly, like the CVD method, template method is also used
energy and structural stability introducing the nitride based MXene to be for the preparation of MXenes where the quantity of obtained MXenes is
dissolved in fluoride-based etchants and hinder their effective etching. larger than the former method. Jia et al. [48] prepared N-doped Mo2C
In the molten salt etching process, these molten salts are producing sheets with MoO2 as the template consisting of perfect crystallinity and
stronger electron accepting ligands, which introducing a thermody morphology. Calcination of MoO2 at 700 ◦ C by dicyandiamide dissoci
namic reaction with A element in MAX phase. Thereby, definite number ates to introduce C and N atoms then it reacts with MoO2 to give N-
of atoms or ions is diffuse to the two-dimensional atomic plane and doped Mo2C sheets. Zhang et al. [49] prepared Mo2C thin films on
introducing a bond with the unsaturated Mn+1 Xn sheet for the pro sapphire substrate by plasma enhanced pulsed laser deposition method.
duction of corresponding MAX phase or MXenes. MXenes produced by Bottom-up methods for the synthesis of MXenes are in a developing
this method are eco-friendly and have a wide number of applications. stage, it needs to be explored more for the preparation of other mono
Immersing MAX phases in the Lewis acid molten salts produces direct layered MXene phases in higher crystallinity and uniformity.
redox coupling of ‘A’ atom with Lewis acid cations introducing the SEM images of MXenes using etching associated synthesis route is
generation of MXene sheets [44]. But majority of molten-salt etching given as Fig. 6. The above-mentioned methods have their own limita
processes are creating MXenes which are not dispersible in water due to tions. Hence, some other new methods are developed for the synthesis of
the deficiency in the –OH terminal groups which make it as hydropho MXenes such as UV-induced selective etching method. Mei et al. [50]
bic, thus it preventing the further processing of MXenes. In the year of prepared mesoporous Mo2C with high quality and high yield from its
2021, Arole et al. [45] synthesized water dispersible Ti3C2Tz MXene Mo2Ga2C MAX phase. Bottom-up methods are usually used for the
using SnF2 as molten salt using Argon flow in a tube furnace in order to synthesis of 2D layered materials but it has its own limitations with its
reduce the contamination due to oxygen. Here the molten salt, SnF2 is low yield and substrate availability. So MXenes are commonly synthe
going to diffuse between the layers in order to form AlF3 and Sn as sized by top-down methods by avoiding the limitations of bottom-up
byproducts with the separation of layers. They further took this pre methods [46].
pared MXene clay for KOH washing, for the production of a stable
MXene dispersion with –OH groups. They found that the molten salt 2.3. Properties of MXene
etching is an effective way for the preparation of MXene phase without
any fluorine content. The pictorial representation of synthesis procedure With the discovery of MXenes from 2011 itself, different experi
followed by them is given as Fig. 8. mental and theoretical approaches are put forward to study their
properties. Brief analysis of the important and basic properties related to
2.2.5. Electrochemical etching charge storage principle of MXene is provided below.
By understanding the health and environmental issues underlying
with the HF assisted synthesis of MXenes, there are some other methods 2.3.1. Electronic properties
are invented. Recently, electrochemical etching is considered as a The electronic and transport properties associated with 2D MXenes
prominent top-down method to prepare MXene from MAX phase by the are widely studied from the theoretical background. Some of the liter
selective extraction of nanolaminate contents such as carbide-derived atures reported that the electronic properties of MXenes are based on
carbon (CDC) and carbon/sulfur with the effective optimization of their composition. By using the GGA framework, the structural and
etching parameters. For example, in the case of Ti3AlC2 the Al layers are electronic properties of MXenes are computed. Hybrid functional is also
etched by the application of constant potential where the chloride ions used to obtain the exact estimation of electronic bandgap. With the
(Cl− ) possess good binding properties with Al and a breakage of Ti–Al existence of strongly correlated d electrons in transition metal elements
bonds. Here the Ti3AlC2 is a positively charged electrode and the chlo a 2 to 5 eV ranging Hubbard correction is applied. MXenes show metallic
ride ions are going to attack it, forming AlCl3with edged Ti atom properties like its MAX phase. The states near to the Fermi level repre
termination and the grain boundaries opening promotes the Cl− pene senting M-d states are produced and the increase in the electrical con
tration and other species are intercalated from electrolytes. Usually, the ductivity of MXenes than its MAX phase is reported. Most of the
surface etching process of MXene from its MAX phase using electro terminated MXenes sustain their metallic behaviour and semi
chemical etching is affected by the presence of protective CDC layers, conductors, such as V2CF2, Sc2CTi2, Ti2CO2, etc., with a Fermi level
and it restricting the bulk scale production via this method. To avoid the shifting [51]. With functionalization, MXenes change their electronic
effect of these protective layers application of intercalants like tetra properties from its metallic to semiconducting phase based upon the
methyl ammonium ion is illustrated, but the toxicity of this intercalants nature of M, X and T groups. Most of the terminated MXenes are stand
is a serious concern. Thus, the application of electrochemical etching by with its metallic nature. –F and –OH terminal groups consisting
thermal assisting is proposed in nowadays [45]. By understanding the MXenes are only accepting one of the electrons from its surface which is
application of thermal assisted electrochemical etching, Pang et al. [44] affecting the electronic properties and – – O terminated groups are
synthesized the MXenes such as Ti2CTx, Cr2CTx and V2CTxin HCl elec capturing two electrons from its surface. So MXenes with group VI; Cr,
trolyte and they found that this method can be applied as a universal Mo, W transitions stand as 2D topological insulators which consist of an
route for the synthesize of HF free MXene in an environmental friendly insulating gap in bulk and gapless states in the edges affected by the
manner, the synthesize procedure and corresponding SEM images are properties. MXene such as Mo2CO2 (M = Mo, W, Cr), M’2M"C2O2 (M’ =
given as Fig. 9. Mo,W; M" = Ti, Zr, Hf) and Ti3N2F2 are stand as semiconductors
7
Fig. 6. SEM images of a) Ti3AlC2 before treatment, b) after HF treatment, Reprinted with permission from [32], Copyright (2012) American Chemical Society. c)
Nb2CTx MXene by treatment with LiF and HCl, d) V2CTx MXene. Reprinted with permission from [33], Copyright (2013) American Chemical Society.
Fig. 7. Pictorial representation of alkali etching of Ti3AlC2 in NaOH solution a) Blocking of Al extraction by Al (oxide) hydroxides in low temperature b) Dissolving of
some quantity of Al (oxide) hydroxides in NaOH under high temperature and low NaOH concentration c) with respect to Bayer process, dissolving of Al (oxide)
hydroxides in NaOH.
Copyright with permission from [42], Wiley-VCH Verlag GmbH&Co. KGaA, Weinheim (2018).
8
Fig. 8. Pictorial representation of reactions takeplace during molten salt etching in a tube furnace in Argon flow.
Reproduced with permission from [45] iScience(2021).
consisting of zero bandgap or as semimetals satisfying the electron and 3. Charge storage mechanisms and different types of
hole Fermi pocket [52,53]. Thin Ti3C2Tx MXene exhibits transparent supercapacitors based on MXene
character and good conductivity which make it as a suitable candidate
for transparent conductive electrodes. A 5 nm thick Ti3C2Tx film usually MXenes are considered as the suitable electrode material for super
transmits about 91.2 % of visible light holding 8 kΩ/sq. resistances and capacitor device applications because of their rapid ion intercalation/
it is possible to take the cation intercalation. Thus, MXenes with metallic deintercalation, faster electron transport, etc. The existence of higher
character are usually applied for the supercapacitor device fabrication number of surface functional groups contributes to the enhanced charge-
[51]. Illustration of electronic band structure of V2C based MXenes are storage mechanism in MXenes. The presence of terminal groups in
shown in Fig. 10. MXene depends upon their physical and chemical properties. Gogotsi
and team reported that MXene having large number of surface func
2.3.2. Mechanical properties tional –O groups exhibit larger surface activity and good pseudocapa
Mechanical properties such as the flexibility of MXenes are highly citive performance [21,22]. With the application of ammonium per
depends upon its industrial applications especially for electrochemical sulfate as weak oxidant and intercalating agent, partially replaced –F
energy storage [52]. Mechanical properties of MXenes are verified by terminating group coupled with controllably oxidizing Ti3C2Tx surface
the theoretical methods based upon the thickness, surface termination produce higher amount of –O terminations [54]. MXenes and their
and composition. In-plane stiffness and out-of-plane rigidity are composites usually act as a negative electrode material because of its
responsible for the elasticity and flexibility in MXenes. 2D MXenes have easier way of oxidation feature in the positive potential. In order to
elastic constants that are two times higher than corresponding MAX enhance its antioxidant performance at positive electrode, preparation
phase. This is due to the presence of extra electrons constituted by N of composite materials with conducting polymer, carbonaceous mate
atoms in accordance with C atoms which points to the generation of rials and its ternary composite is found to be one of the facile and effi
stronger MM-X bonds in nitrides. With respect to the elastic constant cient methods. There are several factors such as synthesis method,
values, 2D transition metal carbides get stiffer if the atomic mass of M morphology, electrolyte, interlayer spacing, etc., are highly affecting the
element increases [51]. Computational studies are also employed for the supercapacitor performance of MXene based devices. In case of MXenes,
study on the effect of terminations in the MXenes elastic properties. the pseudocapacitance is originated from the redox reaction with faster
Presence of terminal groups highly reduces the elastic constant values of intercalation of ions. Thus, higher interlayer spacing will generate more
MXenes. Basically –O terminated systems with smaller lattice param intercalation and favors wide range of electrolytes exposure thereby
eters produce stronger MXenes in accordance with the –F or –OH leading to the improvement in energy density. Sonication or intercala
group terminated MXenes. By using AFM tip for nanoindentation tech tion assisted delamination procedure is found to be one of the suitable
niques the obtained Young’s modulus of Ti3C2Tz is found to be 330I 30 methods to enhance the specific capacitance with the introduction of
GPa, which is lower than the values reported for graphene it’s about cations/large active molecules. Also, the electrochemical performance
1000 ± 100 GPa. Further, along with the lower Young’s modulus in of MXenes is dependent upon the precursors which are used for their
comparison with other 2D materials, large bending stiffness, higher synthesis [21]. From the reported studies by Halim et al. [54], it is found
negative zeta potential, hydrophilicity, etc., make MXenes a suitable that Mo1.33C MXene etched from (Mo2/3Sc1/3)2AlC MAX phase precursor
candidate for flexible energy storage devices [51,53]. induces an increase in specific capacitance by ~65 %. MXenes which are
produced from different HF etching conditions lead to tunable super
capacitor performance. Tao et al. [55] identified that Mo1.33C MXene
etched from its MAX phase (Mo2/3Sc1/2)2AlCshows improved
9
Fig. 9. a) Electrochemical etching procedure of Ti2AlC in HCl electrolyte. SEM image (scale bar 1 μm) of Ti2CTx synthesized in different etching conditions b) un-
etched Ti2AlC, (c) 1 M/25 ◦ C/9 h/0.3 V, (d) 1 M/50 ◦ C/3 h/0.3 V without CB, (e) 1 M/50 ◦ C/3 h/0.3 V, (f) 1 M/50 ◦ C/6 h/0.3 V and (g) 1 M/50 ◦ C/9 h/0.3 V.
Reproduced with permission from [44] Copyright (2019) American Chemical Society.
volumetric capacitance by ~65 % as compared to theMo2C MXene electrodes. By improving the specific surface area of electrodes, it is
without any vacancies. Also, the electrochemical performance of MXene possible to increase their electrochemical performance for super
is depends upon the size of the obtained flakes. MXene with smaller capacitor applications by introducing more accessible sites for charge
lateral size reduces the ion diffusion path, introducing ions in electro storage [55]. With the variation in the synthesis parameters, it is
lytes accessible to the surface of electrode and enhanced electrochemical possible to alter the specific surface area of electrodes, thereby the
performance. But MXene with smaller flakes shows reduced electrical charge storage properties. The introduction of surface defects also im
conductivity with larger value of interfacial contact resistance and de proves the charge storage properties of MXene by the intercalation of
fects, which affecting the supercapacitor performance. Surface func ions and modifies its conductivity. MXenes consist of metallic transition
tional groups attached with the transition metal produce ample active metal atoms and carbon/nitrogen with ceramic properties. The combi
sites for the redox reactions with intercalation of ions which eventually nation of these two elements introduces excellent surface area, better
impact the electrochemical performance. Further, electrochemical per thermal conductivity, good mechanical stability, fascinating optical and
formance of MXene is relying upon the architecture design of the electrical properties with tunability in surface functional groups and
10
Fig. 10. High symmetry configuration electronic band structure of a) V2C b)V2CF2 c) V2C(OH)2, d) V2CF(OH). Zero energy reference represents the Fermi level.
Reprinted with permission from [51], Copyright(2018) American Physical Society.
Fig. 11. Properties of MXenes for supercapacitor applications.
11
Fig. 12. Factors affecting the supercapacitor performance of MXene based electrodes.
intercalation/deintercalation ability. Due to the fascinating electro charge-discharging rate kinetics is more appropriate for the fabrication
chemical properties along with its hydrophilicity, flexibility and 2D of asymmetric MXene based devices [64–66].
arrangement, MXenes emerge as the most suitable material for energy Microsupercapacitors (MSCs) is an alternative for micro batteries
storage devices [56]. The important properties of MXenes for super that got significant attention due to its higher lifetime, large power
capacitor device applications are summarized in Fig. 11. density and rapid charging but the limitation in energy density and
Thus, fabrication of different types of supercapacitor devices such as power density stands as a demerit for the development in microelec
symmetric, asymmetric, micro and hybrid device based on MXenes got tronics. MXenes are considered as a suitable material for micro
tremendous research interest in the current era [57]. 1D symmetric supercapacitors fabrication. But the reduced voltage window for its
supercapacitor device with wire type structure is considered to be an operation stands as a problem. Thus, an asymmetric device fabrication
important wearable and smart microelectronic device. Stainless steel with a pseudocapacitive material is a better choice for it. There are
wires, silver plated nylon fibers like fiber shaped substrates are mainly different techniques illustrated for the fabrication of micro super
used for the fabrication of yarn-based supercapacitors with higher capacitors in sub millimeter scale. Inkjet printing and photolithography
flexibility and good capacitance retention [58–60]. Free standing are considered as a suitable method for the fabrication of micro
MXenes are explored for this purpose by considering several advantages supercapacitors devices [67,68]. Laser scribbling is also a method, a CO2
[61]. Planar structured paper capacitors are developed by loading laser scribbling method was employed by Peng et al. [69] for the
MXene over an A4 paper by laser machining method. Due to the hy fabrication of solid state MXenes supercapacitors, where Ti3C2Tx
drophilic property of MXenes it is possible to use it as the conductive and MXenes is used as the current collector and an active material without
electroactive inks. The prepared inks are stamped, printed, written or any substrate as additive. Microsupercapacitors show good electro
dip coated on to the substrate material for the development of planar chemical performance, stability, flexibility, etc. [70,71]. Xie et al. [72]
electrodes, with improved capacitance retention rate under various fabricated a high voltage microsupercapacitors by simple cutting-
bending conditions demonstrating their good flexibility properties spraying method with Ti3C2Tx MXene as negative electrode and acti
[24,60,61]. 3D structure with open/porous schematics acts as ion vated carbon as positive electrode in PVA/Na2SO4 gel electrolyte. They
buffering reservoirs for the shuttling of electrolyte ions. MXenes pos obtained a higher areal capacitance of 7.8 mF/cm2 with 3.5 mWh/cm3
sessing 3D structure are widely investigated for symmetric super energy density.
capacitors fabrication without any dependence on their small size and With the tremendous attention for smart electronics, the develop
lower stiffness [62,63]. After making an evaluation on symmetric ment of flexible energy devices and products such as smart phone and
supercapacitor performance it is found that the working of MXene is in other devices need robust and flexible transparent conductive electrode
the negative voltage window which stand as a demerit for achieve [73]. Tunable optical properties of MXenes make them as a good
higher energy density, thus for capturing higher energy density, asym candidate for the fabrication of transparent conductive electrodes.
metric device fabrication is reliable. From the reports of MXene based Halim et al. [74] fabricated a Ti3C2Tx transparent film by the selective
asymmetric device fabrication, it is found that usually the system is etching of Al from the sputter deposited epitaxial Ti3AlC2 film. The
assembled with a pseudocapacitive material which is working in the resulting films are possessing a thickness of 19 nm with T = 90 % in
positive window. Organic electrolytes which contain the metal ions such visible-to-infrared regions. Ti3C2Tx aqueous solution is coated on hot
as Li+, Na+, K+ are also used for the fabrication of asymmetric super substrate by Hantanasirisakul et al. [75] produced a transparent ho
capacitors in addition to aqueous electrolytes. The application of mogeneous films holding 5 to 70 nm thickness with 91 % of trans
MXenes for asymmetric device fabrication mainly for non-aqueous mittance. These transparent conductive electrodes based on MXene can
hybrid metal ion capacitors is novel. Providing a wide potential win be prepared in a scalable and cost-effective way. A transparent and
dow with increased specific capacitance without causing any demerits to conductive Ti3C2Tx film is prepared using spin coating method by Zhang
12
13
(caption on next page)
Fig. 13. a) Synthesis procedure for fabrication process of CDs/MXene b)Optical image representing Tyndall effect of d-MXene solution(left) Electrochemical analysis
of material in three electrode-setup c) Cyclic Voltammograms of MXene and hybrid with different mass ratios at a scan rate of 20 mV/s d) CV curve of MXene and
optimized ratio of CDs/MXene-5 % from different biomass sources at 20 mV/s e) Nyquist plot of CDs/MXene-5 % with a magnified curve as inset f) linear fit
representing the relationship between Z’ with ω-1/2 at the low frequency region. Anodic and Cathodic slope values b values of g) CDs/MXene-5 % and h) Pure MXene.
Electrochemical performance of CDs/MXene-5 % i) CV curves at different scan rates j) GCD curves at different scan rates k) cyclic stability performance.
Reprinted with permission from [95] Copyright (2020) American Chemical Society.
et al. [76] and it is applied as a transparent film for symmetric super increases at the edges of MXene sheets with metallic active sites. Maleski
capacitor fabrication, a volumetric capacitance of 80 % is shown by this et al. [29] studied the influence of flake size on the supercapacitor
device. An overview of various MXene based supercapacitor electrodes performance of Ti3C2 flakes. They prepared the MXene flakes by soni
synthesized by different methods is given as Table 1. cation and density gradient centrifugation and found that with the
variation in sonication conditions, the lateral size of MXene is obtained
4. Factors affecting the energy storage performance of MXenes to be in the range of 0.1 to 5 μm. They employed the centrifugation
assisted method to make the MXene sheets with various lateral sizes to
Energy storage performance of the MXene based materials depends monodisperse fractions and obtained a best capacitance value for the
upon several factors as described in Fig. 12. Supercapacitor performance MXene flakes with a lateral size of approximately 1 μm with a value of
of MXenes synthesized through etching process is mainly influenced by 290 F/g at 2 mV/s, which demonstrated that the lateral size largely
the sheet size. It is found that MXene with a large sheet size is suitable as influences the performance.
an electrode material for supercapacitors, but one of the major problems Another important factor which affects the supercapacitor mecha
underlying is the longer etching time of these large sheets [29]. Further, nism of MXene is its morphology. 2D layered MXenes possess a tuned
the longer etching time is found to be not suitable because the capaci morphology. Thickness of the coating is an important parameter for
tance values for these samples are reported to be in the range of 10–20 tuning of the supercapacitor performance. Electrodes based upon
F/g. MXene sheets with a reduced size have the ability to show improved MXenes are commonly synthesized by using coating procedures such as
supercapacitor performance by increasing the amount of electrochemi drop casting over Ni foam or other conducting substrates. Electrodes
cally active sites over the surface in the charging-discharging process. with a thickness in the range of 0.4 mm are usually used for better
With the reduced sheet size, the possibility of oxidation reactions performance of electrode material. Also, MXene with a small lateral
Fig. 14. Pictorial representation of fabrication process of electrode film using electrophoretic deposition; a) sketch and morphology of Ti3AlC2 MXene b) sketch and
morphology of m-Ti3AlC2 c) sketch and morphology of d-Ti3AlC2 e) EPD process and f) sketch and photographs of d-MXene film, MXene-CNT film and CNT film.
Reprinted with permission from [97] Copyright 2018, Elsevier.
14
Fig. 15. CV curve of a) Ti3C2 film b) CNTs film c) Ti3C2/MXene film at various scan rates of GCD curve representing d) Ti3C2 film e) CNT film f) Ti3C2/CNT film g)
Variation of specific capacitance in three electrode system at different current density h)Specific capacitance variation in three electrode system after 10,000 cycles at
5 A/g i) Nyquist plot and inset graph representing the fitted view of equivalent circuit.
Reprinted with permission from [97], Copyright (2018), Elsevier.
dimension produce more ion diffusion thereby the supercapacitor per the edge oriented functional groups are creating oxidation and it
formance. Single and multilayer morphologies of MXenes are suitable significantly affecting the stability of MXenes. From the reported
for energy storage; single layer morphology gives more adsorption/ studies, it is found that the presence of –O functional groups are pro
desorption of ions and an efficient surface area for the accumulation of ducing an improvement in supercapacitive performance than –F func
charges. Also, a multilayer morphology induces higher ion mobility. In tional groups which has the ability to produce hydroxyl bonds
addition to this monolayered and multilayered morphologies, a porous specifically in acidic electrolytes by the protons present in it. From the
structure is also facilitating higher electrochemical performance by the reported studies, it is found that influence of –Cl functional groups in
way of accumulation of electrolyte ions towards its electrochemically the edges and MXene is going to expand its interlayer spaces by the large
active pores and produce better diffusion of ions suitable for the increase ionic radius of chlorine and it is going to produce the faster ion diffusion
in supercapacitor performance [88]. By the method of flash oxidation for supercapacitors. Intercalating molecules is also affecting the super
and hydrothermal oxidation, Naguib et al. [88] prepared Ti3C2Tx and capacitor performance of MXene sheets. Organic/polymer molecule
Nb2CTx respectively with core shell type morphology. They obtained a intercalation to MXene sheets is inducing large interlayer spaces but it is
hybrid of feather like and barrel like morphology for Nb based MXene not as much of sure about the increase in supercapacitor performance
with respect to the change in temperature. Bi-pyramidal and nano because it depends upon the synthesis methods which is followed [59].
cuboids morphology is got for the Ti based MXene. The prepared Ti Supercapacitive performance of every supercapacitor device is de
MXene produced 220 mAh/g with a reversible capacity at C/18 cycling pends upon the electrolyte medium which we are using for analysis.
rate after 30 cycles. Their studies revealed that by varying the synthesis Basically, the electrolytes are of four types; aqueous, organic, ionic and
conditions it was possible to change the morphology thereby the solid. During supercapacitor measurements the electrolytes are held
supercapacitive performance. responsible for the potential window of supercapacitor. In acidic envi
Oxidation of MXenes is found to be as a major problem relating to its ronments the MXene based materials shows higher pseudocapacitive
further exploration. Synthesized MXenes are always contain functional nature which facilitates higher volumetric capacitance. Also, with
groups such as –O, –F, –OH, etc., which produce a chance of oxidation sulfide-based electrolytes like Na2SO4, K2SO4 the material exhibits EDLC
thereby the contamination. Once these MXenes are kept to an open air, behaviour. But for the practical device fabrications, these types of
15
16
Fig. 16. a) Pictorial representation of fabrication of biscrolling MXene with CNT, SEM image representation of b) surface c) morphologies of cross section of
electrode material consists of 97.4 wt% of MXene d) higher magnification colored SEM image with marked portion representing the way in which MXenes are
trapped in the CNT yarn corridors e) SEM image representing the electrode yarn with 90 wt% of MXene tied to a roof knot f) CV curves of cathode and anode material
yarn electrode at 5 mV/s scan rate. CV curves of free-standing yarn supercapacitor analyzed g) in different potential window at 10 mV/s scan rate h) in various scan
rate at 1.5 V i) GCD curve of yarn supercapacitor performed at different current density j) capacitance retention with cycle number for freestanding yarn super
capacitor device k) Ragone plot.
Reprinted with permission from [98], Copyright (2018), Wiley-VCH Verlag GmbH&Co. KGaA, Weinheim.
Fig. 17. a) Pictorial representation for the preparation of MXene-holey graphene film b) CV curve of MXene-holey graphene film based symmetric supercapacitor at
various scan rates c) capacitance retention of symmetric supercapacitor with a current density of 5 A/g for 10,000 cycles, constant current charging-discharging
curves of initial ten cycles and last ten cycle shown as inset d) Gravimetric and e) volumetric energy and power density of MXene-holey graphene based sym
metric supercapacitor in comparison with previous reports. Reprinted with permission from [94], Copyright (2018), WILEY-VCH Verlag GmbH&Co.
KGaA, Weinheim.
17
18
Fig. 18. Schematic representation of pseudocapacitive asymmetric supercapacitor a) synthesis procedure of Ti3C2Tx MXene where surface functional groups are not
shown here due to the sake of simplicity b) Pictorial representation of fabrication process of asymmetric supercapacitor. Panel 1 shows the 3D textured carbon fiber.
Panel 2 and Panel 3 representing the coating of MXene on carbon fiber by drop casting and growth of amorphous RuO2 over carbon fiber by using hydrothermal
technique. Panel 4 giving the representation of RuO2/Ti3C2TxMXene. c) CV diagram of RuO2/CF, Ti3C2Tx/CF asymmetric device at 50 mV/s scan rate. d) CV of RuO2/
Ti3C2Tx asymmetric sandwich arrangement with different scan rate. Inset figure represents the digital photograph of asymmetric device. e) Galvanostatic charge-
discharge curve at various current densities. f) Change in cell capacitance and charge of asymmetric device in current density variation. g) Representation of
normalized real (C’) and imaginary (C”) part of capacitance versus frequency of device. h) Cyclic stability and coulombic efficiency of asymmetric device for 20,000
cycles in 1 M H2SO4 electrolyte at 20 A/g current density. Inset figure shows charge-discharge profiles for first and last charge-discharge cycles i) CV of asymmetric
device with inset figure shows the optical image for in-plane solid state device attaching to polypropylene substrate j) Ragone plot showing areal and power densities
of RuO2/Ti3C2 MXene device in comparison with other devices, where square shape represents carbon-based microsupercapacitors, triangle representing pseudo
capacitive asymmetric device k) CV diagram of RuO2/MXene tandem in-plane device at scan rate of 10 mV/s. Inset figure shows the devices connected in series which
power up a green LED in discharging rate. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
Reprinted with permission from [119], Copyright (2018) WILEY-VCH, Verlag GmbH&Co. KGaA, Weinheim.
conventional electrolytes are not recommended. Commonly, some other choosing a controlled synthesis approach for tuning the interlayer
gel electrolytes like PVA/Na2SO4 are being used. But it possesses mal spaces of MXenes and controlling the amount of surface termina
functions relating to suppression of voltage window collectively the tions. Addition of reinforcements (e.g., bacterial cellulose) with the
reduction in electrochemical performance. Thus, other electrolytes are introduction of interlayer spacing for MXene produces a flexible
also studied, namely, organic and ionic-liquid based electrolytes. electrode for induces good mechanical strength.
Organic electrolytes containing TEBAF4 like conducting salts is dis • A proper theoretical simulation is needed for solving the reason
solving well into the organic solvents such as acetonitrile. These types of behind this induced capacitance of a supercapacitor device. But a
organic solvents have the efficiency to improve the potential window of proper simulation route is not yet explored [90,91]. Thus, the
supercapacitor device than the aqueous ones. But its inherent features formulation of a theoretical method can be done in order to resolve
such as higher cost, toxicity, flammable nature, etc., are stand as a the problems underlying the accumulation of charges to the device.
limitation for its further exploration. Interaction of pores with ionic • Pore engineering in MXene is considered to be an emerging route for
electrolytes stands as a favorable condition for the increase in super research. MXene possesses a brittle like structure thus it is not able to
capacitor performance. EMI-TFSI (1-ethyl-3-methylimidazolium bis- obtain by physical methods, so chemical modification is found to be a
(trifluoromethylsulfonyl)-imide) is a widely using ionic electrolyte, in suitable route [22]. Surface terminations give interesting mechanics
order to verify the performance of MXene in this electrolytes Zifeng et al. such as nanosheet crumbling.
[87,89] performed an experiment in the potential window of − 1.5 to • For MXene based material, the energy storage performance is
1.5 V. They found that in the positive potential the interlayer spacing is depending upon the accumulation of cations between the layers.
going to decrease and it is tending to increase in the negative potential. Thus, the charge storage mechanism in MXenes is influenced by the
Decrease in interlayer space is by the steric effect induced by dein interlayer spaces. So, the introduction of pillaring methods is
tercalation of EMI+ ions and attraction caused by MXene with positive necessary for the increase in interlayer spaces and thereby super
charge and TFSI-anions. They found that in the negative potential EMI+, capacitive performance.
ion intercalation is taken place and increasing the interlayer spaces.
Among this, formation of heterostructure with MXenes is considered
5. Methods to improve the energy storage performance of to be as a major route to enhance its supercapacitor performance. A
MXenes suitable combination of MXene and other guest compounds facilities the
enhanced charge storage activity. The present review mainly focused on
MXene and its heterostructure possess unique features for the charge a detailed discussion about the charge storage in this MXene based
storage mechanism. Multifunctional properties of MXene based mate heterostructure.
rials induce these features for supercapacitor device fabrication. But
there are some limitations associated with this MXene based materials 6. MXene based hybrid materials for supercapacitor
for supercapacitors. It is possible to improve the properties of MXene applications
devices by tuning the chemical constituents, demonstration of nano/
micro structures in order to improve the interlayer spacing. Geometric MXene with interlayer structure, higher surface-to-volume ratio and
flexibility associated with the MXene based nanostructures and availability of electrochemically active sites is producing a favorable
advanced architectures introduce the extraordinary features for super condition for energy storage applications. But it’s restacking and lower
capacitors. Thus, it is believed that MXene based nanostructures and mechanical properties hurdle its further exploration. In order to avoid
modified architectures will introduce a wide variety of opportunities for the difficulties associated with MXene as electrode materials formation
the exploration of upcoming energy storage devices. But its widespread of a hybrid/heterostructure is a suitable and appreciable method for
applications need some material improvement. improves the supercapacitor performance. With respect to its superior
elastic modulus value, tunability of surface terminal groups and higher
• Good conductivity, rate capability, tunable composition, hydrophi aspect ratio make MXene as good filler for composite materials. The
licity and volumetric capacitance introduce significant advantages composites with enhanced properties made the researchers to think
for MXene based supercapacitors. But the stacking and aggregation about the fabrication of flexible, portable and wearable electrochemical
introduces the reduced interlayer spaces and produces inactive en devices. This section discusses about the features of this MXene based
ergy storage kinetics. Therefore, the formation of hybrid composites, heterostructures as electrode material for supercapacitor application.
surface modification and heteroatom doping are considered to be a
route to avoid these problems. Thus, it is necessary to establish some
6.1. MXenes with carbonaceous materials
novel composites/doping elements for the modification of this
MXene based materials.
Currently, the flexible supercapacitor devices have great interest
• Advanced flexibility and self-assembling capability made MXene as a
because of its significant feasibility to deal with the importance of them
versatile unit for constructing supercapacitor electrodes. The energy
in wearable and portable electronic equipment. But the demerits with
storage performance of MXene based electrodes can be optimized by
the development of flexible supercapacitors are its reduced mechanical
19
Fig. 19. a) Preparation process for the fabrication of PDT/Ti3C2Tx film electrode. b) CV curve of symmetric supercapacitor with PDT/MXene film electrode of various
scan rates, c) GCD curve of supercapacitor device with different current density, d) capacitance retention with different bending angles after 100 cycles, e) gal
vanostatic charge-discharge curve of bending angles ranging from 90 to 100 cycles.
Reproduced with permission from [155], Copyright (2018) Elsevier.
20
Fig. 20. Pictorial representation of fabrication process of wavy MXene//rGO/CNT/PANI asymmetric device a) producing Ti3C2Tx and polystyrene dispersion in
water b) with the aid of filtration production of freestanding MXene/polystyrene film c) Production of MXene film by the removal of polystyrene spheres by annealing
d) Compressing the porous film they obtained the wavy MXene film e) GO dispersion in N-Methylpyrrolidine f) By mixing graphene with PANI preparation of rGO/
PANI dispersion g) rGO/CNT/PANI dispersion by the addition of CNT preparation of rGO/CNT/PANI film i) structure of wavy MXene//rGO/CNT/PANI asymmetric
device. j) CV curve of negative and positive electrode at a scan rate of 10 mV/s. k) CV curve of asymmetric device at various scan rate of 10, 20, 50, 100, 200, 500,
1000, 2000, 3000 and 5000 mV/s. l) GCD curve of asymmetric device in H2SO4 gel electrolyte m) Ragone plot of asymmetric device in comparison with other
electrode materials. n) GCD curve of device in PVA/H2SO4 gel electrolyte. o) Digital photo of blue LED in series, inset figure representing the flexible asymmetric
device. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
Reprinted with permission from [159]. Copyright (2020) Elsevier.
21
Fig. 21. a) Preparation of Cu 0.5Co0.5Se2 nanostructures and its application in asymmetric supercapacitor devices b) Pictorial representation of asymmetric
supercapacitor device c) CV diagram of asymmetric device with sweep rate from 10 to 100 mV/s d) GCD curve of asymmetric device at various scan rate e) specific
capacitance with current density variation of device f) cyclic stability of device 10 A/g (inset graph representing the initial and last ten cycles) g)energy density of
device in comparison with other devices.
Reprinted with permission from [173] Copyright (2020) Elsevier.
22
Fig. 22. Lorentzian fits of selected Raman peaks in H2SO4 electrolyte and its changes during charging and discharging.
Reproduced with permission from [204]. Copyright (2016) American Chemical Society.
flexibility. Thus, carbon species like carbon fibers, carbon nanotubes, flexibility and electrical conductivity. The large surface area possessed
carbon aerogels, carbide derived carbon and graphene are proposed as by AC induced and active MXene producing open structure with a
suitable materials for supercapacitor electrode fabrication. Among this, double-layer mechanism clear from the CV and GCD curve, introducing
activated carbon (AC) is widely used because of its higher surface area, a higher capacitance of about 126 F/g with capacitance retention of
pore size, tunability and affordable cost. Yu et al. [92] found that binders 57.9 % at 100 A/g in organic electrolyte greater than pure MXene and
possess an important role for flexibility of devices. They illustrated the polymer bonded carbon films. Currently, the advancement in portable
2D Ti3C2Tx MXene as a flexible and conductive material thereby pre electrochemical supercapacitors needs to be miniaturized and self-
paring MXene bonded flexible carbon electrodes for supercapacitors in powered. Flexible supercapacitor devices got significant interest in
an organic electrolyte with an encapsulation of activated carbon be different fields because of its long cycle life, larger power density, wide
tween MXene layers. For this arrangement, MXene layers induce flexi range of temperature operation and low cost. Fabrication of electrodes
bility, which acted as a crucial candidate for the introduction of flexible possessing good mechanical flexibility is a major parameter for the
electrodes and generates a 3D conductive network to provide the elec electrode demonstration. Activated carbon is primarily used for flexible
tron transport. These activated carbon layers were increasing the dis supercapacitor devices among other carbonaceous materials due to its
tance between the MXene layers thus providing feasible ion and finite microstructure, better packing density, reduced cost and larger
electrolyte infiltrating. They prepared the flexible free-standing film by surface area. Activated carbon is generally used as an electrode material
mixing it with a wafer based colloidal solution of MXene flakes and but it needs polymer binders, usually it occupies about 10 % of electrode
activated carbon then it was vacuum filtered by Celgard 3501 mem mass thereby reducing the energy density of capacitors other than the
branes and found that this procedure is simpler than the conventional contribution to capacitance. But this polymer binder seems to be act as
route of electrode fabrication method with PVDF. MXene nanosheets an insulating material for electricity which turned to be increasing the
acted as flexible and conductive binder producing good mechanical resistance and reducing the device power density. Thus, the
23
Table 1 transportation. Then the heterostructure is shortening the trans

Brief overview of MXene based supercapacitor devices synthesized by different portation of ions and diffusion distance. Thereby the CDs/MXene has
methods. higher volumetric capacitance and cyclic stability. They synthesized this
MXene Synthesis Electrolyte Capacitance obtained Ref heterostructure by coulombic self-assembly procedure and CDs by hy
condition drothermal treatment from wheat straw, enteromorpha prolifera,
Ti3C2Tx Unidirectional H2SO4 213.5 F/g [77] pomelo juice adding to CTAB. Synthesis procedure and electrochemical
films Freezing assisted measurements in three electrode setups are given as Fig. 13. From the
Tape casting CV curves Fig. 13 c) and d) it is clear that some broad peaks are existing
Ti3C2Tx Etching by LiF + H2SO4 372 F/g [78]
in it, with a dominant redox peaks indicating that the charging-
HCl
Ti3C2Tx Electrostatic self- H2SO4 333 F/g at 1 A/g and [79] discharging process holds fast redox reactions introduced by the inter
assembly maintains 261 F/g and calation/deintercalation of protons with the Ti oxidation state change.
132 F/g at 100 A/g and The carbon dot synthesized from pomelo juice has a volumetric capac
1000 A/g itance of 984.5 F/cm3, volumetric energy density of 19.42 Wh/L, rate
Ti3CTx Etching with HCl H2SO4 581 F/g [80]
+ LiF
capacity of 79.80 % and a cyclic stability of 94.6 % after 1000 cycles.
V2CTx 49%HF at 45 h + H2SO4 487 F/g [81] Their studies revealed that renewable biomass can be used as a suitable
TMAOH precursor for stacking and it introduced a new way for CD induced
Mo1.33CTx Etching with 48% H2SO4 339 F/g [55] MXene.
HF for 24 h +
Habib and team synthesized Ti3C2Tx MXene with the doping of onion
TBAOH
Nb4C3Tx Etching with 49% H2SO4 1075 F/cm3 [82] like carbons (OLC) in order to modify the electrochemical behaviour.
HF 140 h + They found that these onions like carbons possess good conductivity,
TMAOH rate handling capabilities and electrochemical behaviour. With the
Mo2TiC2Tx Etching with HCl H2SO4 4137 F/cm3 [83] introduction of OLC to MXene, it is possible to increase the interlayer
+ LiF at 42 h +
spacing and layer stability. Ti3C2Tx MXene is prepared from the bulk
DMSO4
V2C Milder etching H2SO4 209 F/g [84] MAX phase and OLC is by the nano diamond (ND) powder heating. In
with LiF + HCl the CV curve of OLC doped MXene, they got an increase in the area
Mo2.7V1.3 Etching with HCl H2SO4 180 F/cm3 [85] thereby they concluded that the OLC doped sample have higher elec
C3
3 trochemical performance than the pristine. OLC with 5 wt% and 10 wt%
Ta4C3 HF etching H2SO4 413F/ cm [86]
MXene composites are synthesized and the 5 wt% sample have an in
crease in capacitance from 106 F/g to 147 F/g. Physiochemical prop
incorporation of activated carbon and conductive additives for the erties happened between OLC and MXene introducing an enhanced
fabrication of electrodes will improve the electrical conductivity. By supercapacitor performance. Their studies shows that OLC act as a pil
considering this in mind, Li et al. [93] designed a flexible electrode laring support between MXene and prevents its collapse happened after
supercapacitor with Ti3C2Tx MXene as a flexible backbone with acidified large number of charge/discharge cycles hence reducing the number of
activated carbon. By vacuum filtration and vacuum-drying, they ion intercalation pathways [96].
developed a free-standing flexible device with 40 mm diameter in KOH In order to avoid the restacking and to maintain the interlayer spaces
electrolyte. They found that the porosity present in Acidified Activated to facilitate faster diffusion and electrolyte ion transfer, Carbon Nano
Carbon is introducing a faster diffusion path for electrolyte ion tubes (CNTs) have beneficial influence on the MXene based electrodes
charging/discharging process and generate the MXene layer accessi than the pristine one. CNTs are usually mixing with MXene nanosheets
bility to the electrolyte ions, producing good double layer mechanism by dispersion and fussy pre-treatment for MXene and spacers (CNT, rGO,
with a higher specific capacitance of 378 F/g at 0.5 A/g and 88.9 % of etc.) take place. Therefore, a robust and simpler method to hybridize
capacitance retention at 30 A/g. Tian et al. [94] prepared aqueous MXene with spacers was developed by Yang et al. [97]. Here the lab
asymmetric supercapacitors by taking layered Ti3C2Tx as negative prepared 300 mesh Ti3AlC2 was added into a solution of HCl and LiF.
electrodes and Activated Carbon as positive electrodes. They prepared The electrophoretic deposition was carried by using graphite paper as
Ti3AlC2Tx by atmospheric sintering method. For the asymmetric as substrate, connecting to a positive terminal and a large sized graphite
sembly they used fiberglass membrane as a separator and H2SO4 and KBr paper as counter electrode. A constant dc voltage of 8 V for 10 min is
mixture as electrolyte. In the dual ion hybrid supercapacitors this producing an MXene/CNT film over graphite substrate. The synthesis
asymmetric electrode is producing a large volumetric energy density, procedure and corresponding supercapacitor measurements are given as
where the hydronium ion is introduced at the Ti3C2Tx negative electrode Fig. 14 and Fig. 15 respectively. By analyzing the GCD profiles it is clear
and the redox reaction between Br− /B−3 with activated carbon is take that the curves are linear with a small amount of potential drop, and
place in the positive electrode. It shows a larger value of volumetric possessing a triangular shape indicating an efficient electrochemical
capacitance of 250 F/cm3 at 2 mV/s with 102.8 Wh/L volumetric energy behaviour. The prepared electrode has higher specific capacitance of 1.5
density at 428 W/L. The fabricated device has extraordinary cyclic times and 2.6 times greater than Ti3C2 and CNT respectively. They found
stability with 122 % of capacitance retention after 6000 cycles. that the synergistic interaction between MXene and CNT is producing a
Among different carbonaceous materials, Carbon Dots (CDs) got robust structure which enlarging these interlayer spaces. Symmetric
significant interest with its surface defects, chemical stability, accessi supercapacitor device fabricated by this electrode material delivers a
bility for ions and mass, low cost and simple synthesis routes. CDs are maximum energy density of 2.77 Wh/kg at 311 W/kg power density. At
used as guests for composite material because it effectively improves the 5A/g of current density, the energy density reaches to 0.56 Wh/kg with
electron transportation and ion migration with a charging/discharging 416.7 W/kg of power density. The measurement findings revealed that
process, introducing a faster redox reaction and enhancing its specific CNT materials are effective material for enhancing the supercapacitor
capacitance. Li et al. [95] prepared a self-standing film electrode with a performance.
0D/2D architecture by the integration of Ti3C2Tx MXene with CTAB- The small, soft and wearable device preparation in electronics de
CDs. This electrode material is efficiently mitigating the agglomera mands the flexible energy storage device. From the reported papers it is
tion of MXene and CDs. Also, it was increasing the MXene nanosheet possible to demonstrate higher energy density supercapacitors possess a
exposure, benefiting the easily accessible electroactive sites by produc form factor of fabrics that produce good energy solutions with higher
ing MXene layer broadening introducing faster electrolyte ion demand. But the bulkiness makes the conventional fiber shaped devices
with lower flexibility. For the traditional coin cell supercapacitors, they
24
have lower specific capacitance due to its higher weight thus reducing good capacitance retention of 100 % even after 1000 cycles [100]. In
the weight of the loading material motivated the synthesis of spinning order to produce a free-standing assembly, various methods are
electroactive or conductive material into yarn and fibers. Thus, taking employed such as the use of nanostructured conducting spacers, to en
this in mind, Wang et al. [98] fabricated a highly flexible yarn shaped gineer the graphene assembly as a thick film or by create a 3D free
electrode by biscrolling of MXene with CNTs. Addition of CNTs to standing graphene architecture like hydrogels, sponges, etc., the inter
flexible yarns by biscrolling approach introducing a direction for finite connected 2D sheets generate a good electrical conductivity in 3D
integration of active material to CNTs without applying any binder or structure in order to produce a good charge transport.
other additives. Also, in the case of MXene based fiber and yarn it is It is possible to obtain a self-assembly of 3D macroscopic graphene
usually prepared by the coating or wet-spinning approaches. But the hydrogel by a ᴨ-ᴨ stacking interaction of 2D graphene nanosheets with
preparation of electrode material by this approach revealed that the hydrothermal method, the chemical reduction of graphene oxide by the
performance is low. assistance of reducing agent, but the restacking of graphene due to the
Pictorial representations of synthesis procedure and supercapacitor presence of residual oxygen containing group reduce the electronic
measurements are given as Fig. 16. They obtained a volumetric capac conductivity thereby the electrochemical performance. The addition of
itance of 1083 F/cm3 and arial capacitance of 3188 mF/cm2 at 2 mA/ MXene to graphene nanosheets will reduce the restacking [101].
cm2 current density. They also prepared a symmetric and asymmetric Thereby, Fan et al. [102] prepared a flexible and free standing MXene/
device prototype which showed a pseudocapacitive behaviour. The holy graphene modified film by the filtration of alkalized MXene and
symmetric arrangement shows an energy and power density of 8.54 holey graphene oxide dispersions with mild annealing. Alkali content
mWh/cm3 and 530 mW/cm3.For asymmetric configuration they was not only destroying the charge balance of MXene but also provides
employed RuO2/CNT yarn as cathode. the conversion of –F group to a –OH group. The removal of -OH group
They got 61.6 mWh/cm3 energy density and 5428 mW/cm3 power by annealing, increasing the ratio of Ti atoms, which produce a large
density. It produces a good mechanical durability and good performance pseudocapacitive performance. Fabrication procedure of MXene-holey
with this energy storing textile prototype for large number of cycles. graphene film and the results obtained for symmetric supercapacitor
They found that this biscrolling route to create flexible yarn from the arrangement is given as Fig. 17. CV curve Fig. 17 b) shows that majority
delaminated and MXene with pseudocapacitive nature which is get portion of capacitance is generated by the pseudocapacitance originated
trapped in the corridors of helical yarn [79]. from Ti atoms inducing sustaining-reversible redox reaction. The pre
The discovery in the field of graphene in the last decade introduced a pared material has higher volumetric capacitance of 1455 F/cm3 at 2
great achievement in material science. There are many research groups mV/s with capacitance retention of 69 % at 500 mV/s and the fabricated
are studying the application of graphene for the formation of a hybrid symmetric supercapacitor shows higher volumetric energy density of
material with other 2D layered materials. Among all carbonaceous 38.6 Wh/L at 206 W/L power density. Their studies revealed that this
materials, graphene is a suitable material for supercapacitor electrode MXene-holey graphene film symmetric supercapacitor device is with
fabrication because of its high conductivity and it holds higher surface standing its volumetric energy density to a stable level with an increase
area with respect to all carbonaceous materials, for the case of a finely
dispersed solution the specific surface area as 1740 m2/g. But retains
Table 2
this higher surface area of graphene as a solid film is difficult because of Brief overview of electrochemical performance of MXene with carbonaceous
the capillary and van der Waals force which affects these sheets to materials.
collapse and restack under solvent evaporation, thus the use of graphene
MXene hybrid Synthesis Electrolyte Capacitance Ref
in supercapacitors need to be conserve the 2D sheets which should be method
available in a 3D arranged macroscopic structure in multiple length
Nb2CTx/CNT Etching H2SO4 462 mF/cm3 [104]
scales thereby maximize the surface area available to store the charges.
NiMoO4/V2CTx Electrostatic PVA-KOH gel 346 F/g [105]
The influence of graphene to increase the supercapacitor performance of @rGO assembly electrolyte
MXene based electrodes are studied by various groups. Sunil Kumar and Ti3C2Tx/N-doped Facile annealing H2SO4 299.52 F/g [106]
team [99] fabricated a supercapacitor with Ti3C2Tx MXene which is CNT
Ti3C2Tx/ CNT Sonication KCl 515.3 F/g [107]
produced by the etching of Ti3AlC2. They tried to improve the super
Paper composites assisted method
capacitor performance by two methods; firstly, the Ni-foil is used as the MXene/CNT Focused Ion PVA/H2SO4 317 mF/cm 2
[108]
current collector it is modified by the procedure of coating with CVD beam gel
grown graphene. Secondly, they used an ultrafine MXene, which is electrolyte
extracted by the procedure of centrifugation of dark supernatant after Ti3C2Tx/cellulose Vacuum PVA/KOH gel 143 mF/cm2 [109]
nanofiber/ filtration electrolyte
the etching and washing process. They found that the capacitance value
porous carbon
of graphene-based supercapacitor was 1.5 times higher than the film
capacitance without using graphene and obtained a specific capacitance Ti3C2Tx/graphene Laser assisted PVA 54 mF/ cm2 [110]
of 542 F/g at a scan rate of 5 mV/s with a good cyclic stability up to strategy
5000 cycles and higher capacitance retention. MXene with multilayers Ti3C2Tx/rGO Freeze drying PVA-H2SO4 34.6 mF/cm2 [62]
composite and laser gel
have shown an agglomeration and restacking producing a reduction in aerogel cutting electrolyte
surface area, thus exfoliation is a necessary step to exfoliate the multi rGO/Ti3C2Tx films Vacuum KOH 370 F/cm3 [112]
layered MXene to a single layer or few layers. Keliang and team intro assisted
duced a new strategy for the synthesis of MXene-Graphene hybrid. Their filtration
NiCo2N@N-doped Single-step KOH 265 mAh/g [113]
method includes two steps: firstly, the addition of graphite oxide into
Graphene approach (1 A/g)
MXene and the plasma assisted exfoliation of graphite oxide modified 209 mAh/g
MXene. They found that this plasma assisted strategy is avoiding the (50 A/g)
reduction in electrical conductivity and capacitance produced from the Mo2N@carbon-rGO Microwave H2SO4 514.54 F/g [114]
sonication assisted method. For the solid-state supercapacitor fabricated technique
MXene/Graphene Layer-by-layer H2SO4 653.7 F/g [115]
they used carbon cloth as a current collector with PVA-H2SO4 electro assembly
lyte. They found symmetry in charge-discharge curve with a triangular Free standing rGO/ Room PVA/H3PO4 171.4 mF/ [116]
shape indicating an efficient reversibility and capacitive nature of MXene film temperature gel polymer cm2
electrode with a higher specific areal capacitance of 54 mF/cm2 at 0.2 interfacial electrolyte
gelation
A/cm2 with lower resistance value of 13.6 Ω. The prepared material has
25
in volumetric power density when compared with a pure MXene electrolyte with RuO2 as positive electrode and Ti3C2Tx negative elec
supercapacitor device proves that the prepared electrode material is a trode by using minimum intensive layer delamination method for the
promising future device for energy storage as a flexible device. Zhou preparation of MXene. They used the porous textured carbon fabric as
et al. [103,111] fabricated a MXene functionalized and Graphene oxide substrate for loading the electrode material.3D texture exist in carbon
platelets through i–O–C covalent bonding. After GO reduction, there fiber is avoiding the use of binders and produce the adhesion of elec
forms a ᴨ-ᴨ bridging interactions between adjacent rGO platelets with troactive materials, facilitates the increase in active material mass
conjugated 1-amino pyrene-disuccinimidyl substrates, thereby syner loading to a given footprint area. With a comparison to the metal current
gistic interfacial interactions are introduced with ultrahigh toughness. collectors carbon fiber is chemically inert and demonstrated as a suitable
The prepared electrode material has higher volumetric capacitance of choice for depositing a variety of materials. Due to the large conduc
645 F/cm3 at 1 A/cm2 current density with 100 % coulombic efficiency tivity higher proton induced pseudocapacitance makes RuO2 as a suit
and capacitance retention after 20,000 cycles higher than the in able pseudocapacitive candidate for fabricating the supercapacitor.
dividuals. Detailed description of supercapacitor electrodes based on Fig. 18 represents the pictorial representation of synthesis procedure
MXene with carbonaceous material heterostructure is given in Table 2. and its asymmetric device fabrication. The CV and GCD curves of the
fabricated asymmetric device possess a pair of redox peaks which in
6.2. MXene-metal oxide hybrids dicates that the charge storage mechanism developed in this combina
tion is faradaic in nature. The asymmetric device delivers 60 mF/cm2 of
In order to avoid the lower areal capacitance corresponds to the areal capacitance at a scan rate of 5 mV/s and it is maintaining at 50 mF/
MXene and to avoid it from the self-restacking, pseudocapacitive ma cm2 when the scan rate increases to 20 mV/s with the aid of gel elec
terial intercalation is a suitable method. Metal Oxides and MXene hy trolytes. In the asymmetric arrangement of tandem in-plane devices it
brids are considered to be as a suitable combination for high delivered a 3 V of power. The asymmetric device delivered a 37 μWh/
performance supercapacitors. But a proper combination of them is cm2 of energy density with 40 mW/cm2 power density. The device has
necessary to enhance the performance of it. Because here the energy 86 % capacitance retention after charge-discharge of 20,000 cycles. Low
storage is depending upon the surface area and oxidation states, in order cost, non-toxic behaviour, environmental friendliness, higher surface
to modify the performance of metal oxides for supercapacitors, combi area, availability and easy way of fabrication made TiO2 as poor metal
nation of two or more components is necessary. Electrical conductivity oxide candidate for supercapacitor. The TiO2 holds easy way of prepa
in binary oxide is double than the single oxides. Due to this factor re ration in nanoscale range and it is a potential candidate for cost effective
searchers are highly encouraged to prepare a hybrid combination of electrode in supercapacitor.
MXene and metal oxides for enhanced supercapacitor performance. By considering the advantageous of TiO2, Zhu et al. [120] developed
Thus, the zinc based binary metal oxides possess good conductivity, a TiO2 decorated Ti3C2 MXene by in-situ hydrolysis and heat treatment
lower cost and lesser toxicity found to be as better species for higher process. The found a distortion less quasi rectangular shape in CV curve
capacitance asymmetric supercapacitors [117]. By considering the ad with increase in scan rate, indicating the capacitive behaviour and
vantages of metal oxide-based electrode material, Javed et al. [117] higher rate capability of the prepared hybrid and it delivers a specific
fabricated a flexible asymmetric supercapacitor with a battery type capacitance of 143 F/g at 5 mV/s which is found to be 1.5 times higher
bimetallic oxide ZnCo2O4 nano-polyhedra supported on the carbon fiber than the pure MXene. Also, the prepared hybrid material has good
textiles and capacitive Ti3C2Tx/MXene layered component as anode. CV cycling stability with 92 % of capacitance retention even after 6000
curves of the fabricated asymmetric supercapacitor device showed a cycles.
higher level of pseudocapacitive charge transfer nature with a pair of Researchers are found that the low energy density in supercapacitors
redox peaks originated due to the transition between Co2+/Co3+ and the is limiting its further exploration. Thus, there are large number of efforts
GCD curves are also displayed a symmetric behaviour with equal time are put forward to introduce electrode materials which are possessing
for charging and discharging indicates an efficient coulombic efficiency higher surface area, better conductivity and diffusion geometries.
and electrochemical reversibility. The asymmetric supercapacitor de Currently, earth boundary binary metal oxide materials are represented
vice exhibited good charge storage property with 281.25 F/g of higher as a good candidate for the electrode fabrication which possesses good
capacitance at 0.5 A/g with 99.94 Wh/kg energy density at 800 W/kg redox activity and capacitance with wide potential window introduced
power density. Also, the device had good cycle life greater than 99 % by the synergistic effect between pure oxides. Recently, NiMoO4got
after 5000 cycles and better flexibility. Zhang et al. [118] designed a great interest with higher energy storage capacity consists of nickel and
flexible solid-state supercapacitor based on V2O5 and Ti3C2 flake com molybdenum ion to introduce redox reactions but its performance is
posite, here the intercalation was obtained by the addition of CTAB to restacked by the porous structure and inferior conductivities [121]. The
Ti3C2 and V2O5 is introduced into MXene produce a hierarchical struc combination of NiMoO4 with other materials produces good perfor
ture and introduce penetration of electrolyte ions. Electrochemical mance. Based on this, Wang et al. [121,123] fabricated a 2D/2D het
measurements are carried out in the two-electrode arrangement, where erostructure of nickel molybdate and MXene nanosheets with a porous
a Celgard 3501 membrane was used as separator between the composite structure which facilitate the diffusion of electrolyte ions during the
electrodes and two stainless steel plates as current collector and 0.5 M insertion/deinsertion reversible processes and increase its capacitance.
Na2SO4 as electrolyte. CV curves of MXene and CTAB added MXene They found redox peaks in MXene with the presence of nickel molybdate
presented a rectangular shape indicating the electrical double layer indicating the reversible redox process and it was due to the faradaic
mechanism of these components with efficient electron conductivity. reaction happened between Ni2+/Ni3+.At a current density of 0.5 A/g,
But by the addition of V2O5, the CV curve possessed a slight deviation the prepared electrode material possessed 545.5C/g capacitance with
from electrical double layer mechanism by the introduction of small good cyclic stability, due to the synergistic interaction of NiMoO4/
redox peaks, indicating the pseudocapacitive behaviour of the prepared Ti3C2Tx as positive electrode and rGO hydrogel as negative electrode
heterostructure. They obtained a 2065 mF/cm2 of areal capacitance at 3 which achieved about 33.76 Wh/kg of energy density 1.6 V potential
mA/cm2 with 15 mg/cm2 mass loading. Also, it acquired over 93 % of window.
capacitance retention after 6000 cycles at 18 mA/cm2.The solid-state Layered Double Hydroxide (LDH) is found to be as a suitable material
supercapacitor was fabricated by two pieces of rectangular CT- for electrode application. 2D layered LDHs is good candidate with larger
Ti3C2@V2O5 electrode with PVA-LiCl electrolyte and it gave 477 mF/ theoretical capacity because of its structural features with large d-
cm2 areal capacitance at 1 mV/s with various bending states. Jiang et al. spacing property and thin layered structure produce free ion transfer
[119] fabricated an asymmetric device by Titanium Carbide MXene between layers and introduce large surface area and increase the num
which we can able to perform at negative potential in an acidic ber of available sites, but LDHs applications are restricted due to its
26
lower electronic conductivity. The composite material of LDHs with symmetric CV and GCD curve indicating an efficient reversibility of the
MXene promotes the improved capacity for MXene also the LDHs con electrode material. Also, they fabricated an asymmetric supercapacitor
ductivity and cyclic stability. In order to avoid the problem of lower with MoO3-Ti3C2 and nitrogen doped activated carbon as cathode. The
specific capacitance of MXene, Zhang et al. [122] used the benefits of prepared device has volumetric energy density of 48.6 Wh/L, also it
layered double hydroxides (LDHs), where they fabricated a Nickel provides 96.3 % of capacitance retention even after 20,000 continuous
Manganese Layered Double Hydroxide which performs an in-situ charge-discharge cycles. Among various oxides, FeOOH is a good elec
anchoring on MXene sheets by chemical bonds, with the chemical trode material because of its variable oxidation states, low cost and earth
bond assisted interfacial interactions they produced an effective syner abundance. By considering the supercapacitor properties of FeOOH and
gistic effect. The CV curves of the prepared heterostructure showed a Ti3C2Tx, Zhang et al. [127] fabricated FeOOH over Ti3C2Tx nanosheets
redox peak which is due to the Faradaic pseudocapacitive nature of by the facile, low temperature, eco-friendly synthesis procedure. The
material. They obtained a specific capacitance of 1575 F/g at 0.5 A/g electrode material delivered 217 F/g of specific capacitance at 1 A/g of
and a higher cycling stability of 90.3 % after 10,000 cycles at 5 A/g with current density which is greater than FeOOH. Also, it possesses a 64 % of
80 % capacitance retention at 20 A/g. Also, they constructed an asym specific capacitance retention at 12 A/g current density and 81 % after
metric capacitor with activated carbon as negative electrode and its 3000 charge-discharge cycles at 1 A/g. The layered open structure de
mass is about 3 times of positive electrode. The asymmetric arrangement livers high performance. Fe3O4 metal oxide nanoparticles behaved as a
has 169.8 F/g of capacitance at 0.5 A/g with good cycling stability. The negative electrode material for supercapacitor devices due to its higher
device delivered an energy density of 126 Wh/kg at 0.74 kW/kg and theoretical capacitance. Nowadays, Metal Oxide Frameworks (MOF) is
power density 3.3 kW/kg at 97 Wh/kg. Zhou et al. [113] fabricated a used as a good candidate for energy storage and conversion equipment
NiFe-LDH/MXene composite by hydrothermal method and they ob due to its higher surface area, skeletal structure and chemical/functional
tained a 3D porous NiFe-LDH/MXene which delivered 720.2 F/g of properties which are controllable. Xie et al. [128] fabricated a MOF
specific capacitance and its capacitance is retained at 86 % after 1000 derived Co-Fe oxide porous nanorod which was introduced into the
cycles produce a good cyclic stability. A stable sheet-like structure in freestanding MXene film to create the high performing flexible elec
NiFe-LDH and the MXene was introduced and the conductive network trode. MXene acts as a binder and as a conductive additive to Co-Fe
forms a good electrochemical performance which accelerated electron oxide coating which promotes the charge transfer. This porous metal
transport. Thereby the CV and GCD curves were indicating pseudoca oxide introduces a feasible ion transmission path for MXene and it re
pacitive behaviour. Also, the asymmetric supercapacitor constructed lieves the electrode material stress with a charge-discharging process.
with NiFe-LDH MXene as positive electrode and activated carbon as This flexible Co-Fe oxide/Ti3C2Tx composite paper withheld 2467.6 F/
negative electrode gave 758.27 W/kg of power density at 42.2 Wh/kg cm3 of volumetric capacitance in 1 M LiCl electrolyte. Also, it introduced
energy density. Battery type binary metal oxides were used in the 88.2 % of high capacitance retention after 10,000 cycles with good cy
fabrication of hybrid supercapacitors because of its large theoretical clic stability. By considering the advantages of Fe3O4 and rGO, Arun
capacitance, higher electrochemical activity, multiple oxidation states et al. [129,130,133,134,145] fabricated a hybrid composite of MXene/
and bulk redox characteristics. Bimetallic hydroxides also possessed a Fe3O4/rGO, the Fe3O4 is decorated MXene nanosheet was generated on
layered structure comparable to MXene. In this type of materials, the the rGO by chemical oxidation method. The prepared ternary composite
interlayer anions were adjustable and they have found profound interest is employed as negative electrode and the capacitive performance is
in electrochemical properties. Wu et al. [124] fabricated a 2D in evaluated on choosing KOH, Na2SO4 and LiCl as electrolytes. From the
terstratifications assembly hybrid electrode with the electrostatic as evaluation of electrochemical performance, they found that the elec
sembly of CTAB modified MXene and dodecyl benzene sulfonic acid trode material shows better behaviour with LiCl electrolyte with
anion modified Ni Co-LDHs. Self-restacking in the MXene and Ni Co- capacitance retention of 82.1 % after 5000 continuous charge-discharge
LDHs can prevent production of an interstratifications structure and cycles at 5 A/g. The preparation of MXene-TMO heterostructure is in the
interlayer spacing, thereby it introduced an electrolyte ion diffusion and developing stage and an overview of the supercapacitor electrodes
carries a large number of electrochemically active sites. In a three- fabricated with MXene/TMO heterostructure till now is given as Table 3.
electrode system this electrode material delivered 1207 F/g specific
capacitance at 0.5 A/g scan rate with good cyclic stability and 93 % of 6.3. MXene-polymer hybrids
capacitance retention even after 5000 cycles possessing a pseudocapa
citive nature. The prepared material had 107.3 Wh/kg energy density at In the case of traditional carbon-based electrochemical capacitors
571 W/kg power density in an aqueous electrolyte. Transition Metal there exists a demerit such as its resistive nature at frequencies which
Magnite (MnO2) based materials were found to be as good positive are above 1 Hz, which limits their widespread applications. Due to the
electrodes due to its natural abundance, low cost and higher theoretical evolution in the field of wearable electronic devices, supercapacitors
capacitance than other oxide materials. By using the advantages of with higher flexibility and cyclic stability are needed in order to
MnO2, Chen et al. [125] fabricated an asymmetric supercapacitor with demonstrate it for real-time applications. With respect to other pseu
K+/Na+ inserted on MnO2 on Ni foam as positive electrode and layered docapacitive elements, conductive polymers such as Polyaniline (PANI),
Ti3C2Tx paper on Ni foam as negative electrode. The pseudocapacitance Polypyrrole (PPy) and Poly (3,4-ethylene dioxythiophene) PEDOT are
of MnO2 is mainly depends upon the quantity of pre-inserted cations. got attention because of its facile synthesis, better conductivity, good
Also, 2D MXene is a negative electrode for supercapacitors because of its flexibility and higher redox activity. The applications to conductive
surface tunability, hydrophilicity and metallic conductivity. 2D nano polymers itself produce large degree of volumetric swelling and
structure possesses large surface area and faster electrolyte penetration/ shrinking so it is used as an additive to most of the supercapacitor ma
diffusion due to less Ostwald ripening and aggregation and the nano terials especially with 2D layered materials to increase its capacitive
sheets avoid the breakage of materials. Here the GCD curves are showed performance. In order to avoid the demerits of these conventional
a triangular shape in different current densities indicating the efficient carbon-based capacitors, Gund et al. [153] fabricated a synergistically
rate performance and reversibility of the prepared electrode material interacting Ti3C2/poly (3,4-ethylene dioxythiophene)-Polystyrene sul
and it was in agreement with CV curve. The asymmetric supercapacitor fonate hybrid by spray coating method. By changing the composition
device had 249 mF/cm2 areal capacitance with 9.39 mW/cm2 power and thickness of hybrid films they fabricated the solid-state electro
density 0.11mWh/cm2 maximum energy density and good cyclic sta chemical device for AC filtering. The prepared composite which is Au-
bility. Zheng et al. [126] fabricated a supercapacitor based on MoO3 coated PET in 3 M H2SO4/PHEMA/PVA gel electrolyte, introduced a
mixing with Ti3C2 in a 5 M LiCl electrolyte, introduced a 631 F/cm3 at 1 specific capacitance of 0.56 F/cm3 at 120 Hz mF/cm2. This electrode
A/g volumetric capacitance and 474 F/cm3 at 10 A/g with a near material maintains its capacitance up to 1000 V/s due to the MXene-
27
Table 3 layer and faradaic charge transfer mechanism. They found that the PANI
Brief outlook of MXene/TMO heterostructure as electrodes for supercapacitor. incorporated material have capability to perform in a 1.45 V voltage
MXene/TMO Synthesis method Electrolyte Capacitance Ref window with higher energy density of 17 Wh/kg with 88 % of capaci
used value no tance retention after 20,000 cycles in 3 M H2SO4 electrolyte. With
CTAB- Etching followed by Na2SO4 477 mF/cm3 [118] respect to the flexibility and compatibility, conjugated polymer elec
Ti3C2@V2O5 annealing trodes got significant advantages, because of its intrinsic conductivity
Ti3C2/TiO2 Microwave KOH 102.5 F/g [131] and film formation property. But these straight chains like conjugated
oxidation polymers possess higher volumetric swelling and shrinking in the
Ti3C2/WO3 Hydrothermal H2SO4 566 F/g [132]
electrostatic
charge-discharge process. Also, this conjugated polymer electrode has
absorption large capacitance loss after cycling/bending test. Thus, it forms the
NiMoO4/Ti3C2Tx Hydrothermal and KOH 545.5C /g [121] demerits of straight chain conjugated polymer electrodes. By consid
post calcination ering this in mind, Wu et al. [155] fabricated a free standing decen
NiMn-LDH/Ti3C2 In-situ KOH 1575 F /g [122]
tralized conjugated polymer (PDT) with layered Ti3C2Tx. They
crystallization
NiFe-LDH/Ti3C2 Hydrothermal KOH 720.2 F/g [135] fabricated the uniform PDT/Ti3C2Tx film with 2,6-dimioanthraquinone
method (DAQ), tetrakis (4-bromophenyl) methane (TM) and Ti3C2Tx by Buch
Ti3C2/Ni-Co-Al- Liquid phase co- KOH 748.2 F/g [136] wald Hartwig coupling. The conjugated polymers possessing decen
LDH feeding and tralized chains increased the contact area with MXene nanosheets and it
electrostatic
attraction
avoided the volumetric swelling and shrinking by the charge-discharge
MXene/MoO3 Vacuum filtration H2SO4 545 F/g [137] process introducing increased specific capacitance and cyclic stability.
Ti3C2Tx-MoO2 Vacuum filtration LiCl 63 F/cm3 [138] They prepared the free standing MXene/PDT film by coating the ac
MnO2@Ti3C2Tx- Hydrothermal Na2SO4 181.8 F/g [139] cordion structure MXene over the FTO substrate. By peeling this film
CNT method electrolyte
from FTO substrate they obtained the free-standing film and analyzed its
MnO2/Ti3C2Tx/ Hydrothermal KOH 511.2 F/g [140]
Carbon cloth method performance in a three-electrode system using H2SO4 as electrolyte and
Ti3C2Tx confined Confinement of Ionogel 172.49 F/g [141] obtained a specific capacitance of 284 mF/cm2 at 0.5 mA/cm2 current
Mn-Fe MnFe2O4 nanodots electrolyte density. The symmetric solid-state supercapacitors fabricated by this
bimetallic (MFNDs) in electrode deliver 52.4 mF/cm2 of capacitance with good flexibility in the
oxide hierarchically
dynamic/static bending cycles. Here the CV curve of fabricated elec
layered Ti-MXene
(Ti3C2TX) trode material shows a closed structure and GCD curves possess a
CoOx-NiO/ Atomic Layer KOH 1960 F/g [142] triangular shape which indicates the double layer mechanism with
Ti3C2Tx Deposition higher reversibility delivers higher capacitance. After 100 dynamic cy
Co3O4 Doped3D In-situ reduction KOH 345 F /g [143]
cles, the device attained a capacitance retention reaches to 96 % with
MXene/RGO and thermal
annealing process good flexibility. The strong bond exists between the functional groups of
Co2NiO4/Ti3C2Tx Hydrothermal KOH 719.5 F/g [144] PDT and rigid MXene sheets are restricted and the rigid MXene sheet is
method strengthening the polymer backbones, thereby producing a good cyclic
Ti3C2/Ni-Co-Al- liquid phase co- KOH 748.2 F/g [136] stability and charging-discharging process. The procedure followed by
LDH feeding and
them is given as Fig. 19. By using the one-pot/in-situ polymerization of
electrostatic
attraction Polyaniline monomer over Ti3C2 nanosheets in an organic acid solution
NiCo2- Hydrothermal and KOH 240 F/g [146] like malic acid/tartaric acid, Wu et al. [156] fabricated a hierarchical
LDHs@MXene wet chemical Ti3C2 nanosheets/Polyaniline nanotube. The MXene component pro
method
duced good mechanical stability, higher conductivity and availability of
MnO2/Ti3C2Tx/ Intercalation and Na2SO4 851 F/cm3 [147]
rGO delamination
more active sites and PANI acts as a 1D high speed transport channel
Ti3C2Tx-MoO2 Vacuum filtration PVA-LiCl 63 F/cm3 [148] which modifies the contact area of electrode and ion acceleration and
Electrostatic KOH 253 mAh/ [149] pseudocapacitance. They obtained 596.6 F/g of specific capacitance at
MXene/ assembly approach cm3 0.1 A/g with 94.7 % of capacitance retention after 5000 cycles. Also, the
Bi2.88Fe5O12-x
symmetric supercapacitor assembly possessed 25.6 Wh/kg energy den
WO3/Ti3C2Tx Electrostatic H2SO4 297 F/g [150]
attraction sity at 153.2 W/kg power density with 1 M H2SO4electrolyte. Their re
NiO/ Ti3C2Tx Hydrothermal KOH 92.0 mAh/ [151] sults demonstrated that the prepared conducting polymer incorporated
method cm3 material is a suitable electrode material. Zhang et al. [157] proposed a
Ti3C2Tx/rGO/ Hydrothermal PVA-KOH 2.32 F/cm3 [152]
unique structural design of 3D architecture with Polypyrrole nanofiber
NiCo2O4 method
and MXene sheets dispersed in Polyvinyl alcohol (PVA) matrix. 1D
structure of PPy nanofiber and 2D property of MXene sheets are
polymer hybrid synergistic interaction, with a near rectangular shape in increasing the mechanical properties of hydrogen hosts. The fabricated
CV curve and it was in agreement with the GCD curves indicating the hierarchical structure promotes the diffusion of electrolyte ions with
double layer mechanism and it provides a device flexibility and dura advanced capacitive properties. The CV curve of prepared hetero
bility over 30,000 cycles. Muhammad Boota and Yury Gogotsi [154] structure showed a quasi-rectangular shape which indicating the double
fabricated an asymmetric supercapacitor with 2D Ti3C2Tx as cathode layer mechanism and the GCD curve showed a symmetric and linear
and conducting polymer (PANI, PPy and PEDOT) deposited over rGO pattern pointing to the highly reversible faradaic reaction. The fabri
sheets by oxidative polymerization as positive electrode. The prepared cated electrode material delivers specific capacitance of 614 F/g at 1 A/
supercapacitor material delivers good energy and power density. In the g current density with 100 % capacitance retention after 10,000 cycles
CV curves of asymmetric supercapacitor device fabricated from PANI and 99.6 % of coulombic efficiency. This large capacitance value is due
and PPy heterostructure shows a reversible redox peak, but the PPy to the higher electrical conductivity of PPy introducing a pathway for
based device delivers broadness in the oxidation and reduction peaks. A transfer of electrons. Also, the PPy with nanofiber structure act as a
stable pseudocapacitive character is found in PEDOT based device conductive bridge to MXene nanosheet promotes electrochemical reac
indicating the phenomenon of easily accessible proton transport. CV tion. PVA hydrogen with porous network introduces diffusion of ion and
curves of these polymer-based devices shows a combination of double its exchange by the active interface between electrolyte and electrode
materials. Also, the hydrophilic nature and elasticity of hydrogel is
28
producing the electrodes to perfectly attaching the hydrophilic carbon H2SO4 and 86.7 mF/cm2 in PVA/H2SO4 solid state electrolyte at 1.5
cloth current collector producing stable and faster electrochemical mA/cm2 current density. The planar Ti3C2Tx/PPy is synthesized by laser
process with reduction in charge and mass diffusion resistance. ablation in order to prepare an interdigital pattern by etching over the
Qin et al. [158] fabricated a flexible solid-state supercapacitor with ITO glass. Then they deposited the Ti3C2Tx flakes over ITO glass surface
vacancy ordering in a layered MXene/Poly (3,4-ethyl by electrophoretic deposition at a 30 V potential for 2 min, then by
enedioxythiophene): Poly (styrenesulfonic acid) with concentrated electrochemical polymerization with 0.8 V potential they deposited PPy
H2SO4.This flexible solid-state supercapacitor produces 568 F/cm3 on Ti3C2Tx/ITO by electrochemical polymerization by chro
maximum capacitance and 33.2 mWh/cm3 energy density and 19,470 noamperometry method. GCD curves of the prepared electrode mate
mW/cm3 power density. There exists a synergistic interaction of va rials show nearly isosceles triangles without any redox peaks indicating
cancy ordered MoC MXene layer with the insertion of conductive PEDOT the highly capacitive nature. The planar supercapacitor has 3.398 μWh/
with a nearly triangular GCD curves which indicating the reversibility of cm2 of areal energy density at 0.0845 mW/cm2 power density and at a
redox reaction and an efficient coulombic efficiency of the prepared 0.338 mW/cm2 power density, it gives 2.028 μWh/cm2 energy density.
hybrid. By using the energy storage properties of CNT, MXene and PANI, Also, the planar device delivers 96 % capacitance retention after 10,000
Li and team [159] prepared an asymmetric supercapacitor with Ti3C2Tx cycles. They verified the practicability of the device by the connected
MXene as negative electrode and rGO/CNT/PANI as positive electrode. solar cell. Conjugated Microporous Polymers (CMPs) are considered to
By mechanically compressing the 3D porous MXene film they prepared be as a fascinating organic porous material fabricated by rigid covalently
the wavy MXene electrode. They made a comparison with other tradi bonded molecules in a 3D network skeleton arrangement. In comparison
tional methods of preparation of MXene film; they found that this wavy with traditional polymersit is possible to synthesis CMP with different
pattern of MXene film produces efficient ion transportation so it is very method in a low-cost method got significant attention in energy storage,
capable to deliver higher capacitance value. By using molecular level catalysis and gas sensing. Yang et al. [162] fabricated MXene based
integration of PANI on graphene with further introduction of CNT, they conjugated microporous polymers by using p-iodophenyl functionalized
produced the positive electrode for asymmetric arrangement, this MXene as template. The MXene based conjugated microporous polymer
sandwich-like structure producing an enhanced ion transportation rate possesses 2D structure and has higher surface area. Also, it avoids the
and the utilization of PANI on this positive electrode. Open structure and restacking and oxidation of MXene. The prepared electrode material has
compatibility of negative and positive electrodes introducing a higher higher specific capacitance than the individual materials. This incre
performance for supercapacitors. Pictorial representation of fabrication ment is due to the advantages of individual materials which combine the
procedure and supercapacitor measurements with device fabrication is MXenes electrical conductivity and the abundant active sites of conju
given as Fig. 20. From the CV and GCD curves it is clear that the fabri gated microporous polymer. There are different combinations of
cated device possesses a pseudocapacitive behaviour and it delivers a MXene/conducting polymer heterostructure based electrodes are fabri
volumetric energy density of 70 Wh/L at 11 kW/L power density and cated; an outline on the supercapacitor studies done with this hetero
63.5 Wh/L at 34.3 kW/L in PVA/H2SO4 gel electrolyte. structure is given as Table 4.
Jian et al. [160] designed a carambola like MXene -Polypyrrole
composite by one-step co-electrodeposition method. The MXene act as a 6.4. MXene-TMDs hybrids
core polymer due to the presence of functional groups (–F, –OH or
–O) into their surface and monomer radical cation on pyrrole monomer
The application of nano spacers through various layers increases the
is introduce a surface polymerization thereby the 2D structure produce a surface area of MXene. Transition Metal Sulfides are promising material
3D structure with good electron transfer and diffusion of ions. It pro for energy storage application because of its large theoretical capaci
duced 416 F/g of gravimetric capacitance at 0.5A/g. The CV and GCD tance, better electrical conductivity, availability of raw materials and
curves showed pseudo-rectangular and symmetric triangular shapes reduced environmental pollution. Transition Metal Dichalcogenides
which pointing to the reversible charging/discharging process and (TMDs) is a good option to improve its specific capacitance, basically to
higher capacitive behaviour. The symmetric supercapacitor fabricated avoid its tendency for bonding to hydrogen or the reduction in capaci
by ITO glass coated by MXene/PPy composite produced 184 F/g of tance by van der Waals force. By considering this, Vyskocil and team
specific capacitance at 10 mV/c with 86.4 % capacitance retention at [171] fabricated a supercapacitor by Ti3C2 MXene prepared by the se
5000 cycles at 5 A/g with good cyclic property. Nowadays, planar lective etching of aluminum layers with tetrabutyl ammonium hydrox
supercapacitor device got tremendous attention in the field of elec ide with ultrasonically synthesized 1 T Tungsten Disulfide (WS2) nano
tronics due to its portability, flexibility and safety. Zhang et al. [161] spacers. They optimized the ratio of 1 T phase WS2 to Ti3C2 as 10 %:90
fabricated a planar supercapacitor device with Ti3C2/PPy synthesized by %. By 10 % of WS2 addition, the gravimetric capacitance is increased
electrophoretic deposition and electrochemical polymerization. In the from 23.3 F/g to 28.2 F/g with a double layer mechanism. Through
three-electrode setup, the electrode delivered 109.4 mF/cm2 in 2 M insertion, there are large number of active sites are introduced. Cobalt
Table 4
Brief outlook of MXene/conducting polymer-based materials as electrodes for supercapacitor.
MXene/CP Synthesis method Electrolyte Capacitance Ref
no.
Polypyrrole@bacterial cellulose/Ti3C2Tx In-situ polymerization of PPy on BC followed by H2SO4 236 F/g [163]
assembling it to MXene
MXene–polyoxometalate (POM) nanohybrid using poly (ionic liquid) Electrostatic interactions with self-assembly H2SO4 384.6 F/g [164]
(PIL) as the linker approach
Mo 1.33 C/poly(3,4-ethylenedioxythiophene): poly (styrenesulfonic Solution processing H2SO4 568 F/cm3 [165]
acid) (PEDOT: PSS) composite film
3
Polyaniline nanodot decorated Ti3C2Tx Simple blade coating H2SO4 1167 F/cm [166]
PPy/Ti3C2Tx film Vacuum-assisted filtration and electrochemical PVA/H2SO4 gel electrolyte 420.2 F/g [167]
deposition
Ti3C2Tx@PEDOT In-situ polymerization H2SO4 564 F/g [168]
Polyaniline nanofiber/MXene film Layer-by-layer assembly LiClO4 dissolved in 17.6 μAh/ [169]
propylene carbonate cm2
Polypyrrole MXene coated textile electrode Dipping-coating assisted method H2SO4-PVA gel electrolytes 343.20 F/g [170]
29
sulfide is a promising material among different sulfides because of its firstly adsorbed over Ni foam using electrostatic assembly. MXene and
lower electronegativity, better electrical conductivity, large specific Ni3S2 promote the charge transfer and increase the electrochemical
capacitance and availability of redox active sites. But due to the volume performance and stability in a faradaic charge transfer process. The
change during redox process which decreases its cyclic stability and rate hybrid supercapacitor consists of Ti3C2/Ni3S2/Nickel foam as positive
capability and it is not conductive to the applications. In order to electrode and active carbon as negative electrode. This hybrid device
improve the specific capacitance of cobalt sulfide and MXene, Liu et al. promotes 66.5 F/g specific capacitance at 0.5 A/g with 76.3 % cyclic
[172] prepared a hybrid of these two materials where the CoS2 is stability after 5000 cycles at 1 A/g. The device delivers 23.6 Wh/kg
fabricated over MXene by one step hydrothermal method. CoS2 is energy density at 4004.4 W/kg power density in 6 M KOH electrolyte.
introducing large number of metal ions active sites over MXene. In a Among different transition metal sulfides Ni–Co binary metal sulfide
three-electrode arrangement they got a specific capacitance of 1320 F/g possess higher specific capacitance with redox reactions and good
at 1 A/g current density with good cyclic performance of 78.4 % after electronic conductivity. Jiang et al. [177] fabricated a Ti3C2Tx MXene
3000 cycles at 10 A/g with small redox peaks in the CV curve and a non- nanosheet wrapped on NiSe2 by hydrothermal method. Due to the
linear behaviour in GCD curve points to the pseudocapacitive nature. higher interfacial interaction of NiSe2 and MXene the three-electrode
The prepared asymmetric supercapacitor with prepared composite as system with KOH electrolyte delivers 531.2 F/g specific capacitance at
positive electrode and reduced graphene oxide as negative electrode in 1 A/g with excellent cyclic stability. Among different transition metal
1.6 V potential window delivers 28.8 Wh/kg higher energy density at sulfides, Ni–Co binary metal sulfide possesses higher specific capaci
800 W/kg power density. It maintains capacitance retention of 98 % tance with redox reactions and good electronic conductivity. By using
after 5000 cycles at 5 A/g which promotes its application in super this property, Li et al. [178] prepared a chrysanthemum like NiCo2S4 on
capacitors. From the reported papers it is found that metal selenide MXene by hydrothermal method. The fabricated asymmetric super
electrode materials have good electrochemical properties because of its capacitor device with prepared material act as positive electrode and
large surface area, porous network structure and good electrical con activated carbon as negative electrode it delivers 621 F/g specific
ductivity. Basically, the cobalt-selenide based materials are introducing capacitance at 0.5 A/g with 72.82 Wh/kg energy density at 0.635 kW/kg
good cyclic stability but its specific capacitance is low. The bimetallic power density. There is only few reports based upon the fabrication of
CuCoSe TMCs have good electrical conductivity with large number of electrode material based on TMD and MXene [185] heterostructure and
redox reaction kinetics holding fascinating electrochemical properties. an overview of the works based upon this combination is given as
Based on this by considering the charge storage property CuCo TMCs, Table 5.
Dakka and team [173] fabricated an asymmetric supercapacitor device
by taking Cu0.5Co0.5Se2 as positive electrode and Ti3C2 as negative
6.5. MXene with other sulfide hybrids
electrode. CuCoSe2 is prepared by a series of hydrothermal and subse
quent selenization processes in order to improve the electrochemical
It is possible to modify the energy storage properties of MXenes by
performance. This asymmetric supercapacitor device delivers increased
the surface modification of it with other pseudocapacitive materials.
specific capacitance from 33.5 to 236.72 F/g by changing the potential
Combination of two materials provides higher specific capacitance.
window from 0.6 to 1.6 V using PVA-KOH gel electrolyte with NKKTF40
Ternary metal sulfides deliver higher conductivity than TMO because of
as separator. With the increase in the potential window, the asymmetric
its strong covalent nature. Wu et al. [188] says that the MXene decorated
device shows complete oxidation and reduction peaks which indicating
with NiCo2S4 nanosheets have its own disadvantages originated by the
the efficient reversibility with good electrochemical performance of
reduced surface area of Ti3C2 and disadvantages with NiCo2S4.Thus,
prepared electrode material. These selenium-based nanostructures have
they prepared 3D hierarchical nitrogen doped Ti3C2-NiCo2S4 nano
unique structure, higher specific surface area, porous structure and
composites, where NiCo2S4 is prepared by hydrothermal route anchored
excellent conductivity which boost the performance of MXene with its
on the exfoliated ultrathin nitrogen doped MXene sheets by in situ
synergistic interaction. At 0.604 kW/kg power density, it delivers 84.17
nucleation and ion exchange reaction. The prepared heterostructure and
Wh/kg energy density with good cyclic stability of 91.1 % of 10,000
the interfacial friendly interaction between two compositions not only
charge-discharge cycles. Pictorial representation of fabrication process
provide the conductive substrate but large number of electroactive sites
and measurements are given as Fig. 21. By using a surfactant assisted
and larger electrochemical storage capability. The electrode delivers
interstratifications process Kirubasankar and team [174] synthesized
1849 F/g specific capacitance at 2 mV/s with lower internal resistance,
the heterogeneous 2D layered MoS2/Ti3C2 hybrid for asymmetric
supercapacitor. The prepared material acts as an anode and β-Ni (OH)2
Table 5
as positive electrode with KOH as electrolyte. The CV curve of the pre
Brief overview of MXene/sulfide hybrid for supercapacitors.
pared electrode material shows non-ideal triangular behaviour of both
EDLC and pseudo with a good reversible nature and the GCD curve is in MXene/sulfide Synthesis method Electrolyte Capacitance Ref
hybrid no.
agreement with it. The fabricated electrode is arranged in a three-
electrode combination, which delivers 583 F/g specific capacitance at Ti3C2Tx/CoS2 Solvent thermal KOH 1320 F/g [179]
1 A/g with 82.5 % of rate capability and 96.5 % cyclic stability at 5 A/g method
VS2/MXene Hydrothermal K2SO4 115.7 F/g [180]
in 5000 cycles. Method
The asymmetric devices give 153 F/g specific capacitance at 1 A/g NiS grown on Hydrothermal KOH 857.8 F/g [181]
with 90 % capacitance retention in 10,000 cycles at 5 A/g. The device Ti3C2TX method
has 54 Wh/kg energy density and 0.86 kW/kg power density. By wet MXene/ Two step KOH 1165 F/g(1:5 [182]
NiCo2S4 hydrothermal method %)
impregnation of MoS2 on MXene, Mijun Chandran and team [175]
VS2 / Ti3C2Tx Hydrothermal KOH 88.1 F/g [183]
fabricated a symmetric supercapacitor device in H2SO4 electrolyte it method
gives 342 F/g specific capacitance at 0.4 A/g with greater than 99 % of MoS2-Ti3C2Tx Hydrothermal H2SO4 115.2 F/g [184]
discharge time which retained after 10,000 cycles, this higher perfor method
mance in this enlarged window from − 1.5 V to 1.5 V is due to the NiCo2S4/ Hydrothermal KOH 621 F/g [178]
MXene method
reduction in equivalent series resistance of MXene by MoS2. Zhao et al. Ti3C2Tx Hydrothermal KOH 531.2 F/g [186]
[176] fabricated a 2D layered heterostructure of Ni3S2/delaminated MXene/ method
Ti3C2 which is supported on the Ni foam for a binder free electrode for NiSe2
hybrid supercapacitor. With solvothermal method they synthesized CuS/Ti3C2 Hydrothermal KOH 169.5C/g [187]
method
Ni3S2 using Ni foam as nickel source and substrate, before that Ti3C2 was
30
good rate performance and better cyclic stability in KOH. Li et al. [189] non-linear discharge curve present in GCD shows a pseudocapacitive
fabricated a 3D NiCo2S4 on Ti3C2Tx based Nickel foam for binder free nature which is due to the surface redox reaction of the prepared com
electrode. The synthesis involves the co-electron deposition of mixed Ni, posite in the electrode/electrolyte interface. Dodecaborate is a novel
Co metal hydroxide precursor followed by vapor phase hydrothermal photoelectric material due to its B–B bond it creates an icosahedral cage
method. They fabricated an asymmetric supercapacitor with prepared conjugate structure with its electrons of dodecaborate ions is strongly
material as positive electrode and activated carbon as negative electrode delocalized in 3D ᴨ bond structure with its negative charge produce a
in PVA-KOH polymer electrolyte. In a three-electrode system, it delivers delocalization over dodecaborate ion produce a reduction in probability
596.69C/g of specific capacitance at 1 A/g with 80.4 % capacitance to cation binding. With respect to its good optical and electrochemical
retention after 3000 cycles at 10 A/g. The asymmetric supercapacitor behaviour borate is mostly used as solid electrolyte for energy storage
consists of activated carbon@nickel foam as negative and prepared device in order to reach large power density and stability. By using the
material as positive electrode. Due to MXenes faster ion transport and features of dodecaborate and MXene, Li et al. [194] fabricated a highly
the interfacial contact generated by the electrolyte and active material conducting dodecaborate/MXene composite by the modification of
by Ni2Co2S4 nanosheets and AC@NF facilitates the ion transport and MXene surface by simple ultrasonic treatment with addition of ammo
electrolyte produce reduced resistance collectively benefiting to pro nium ion and an insertion of dodecaborate ion to the MXene inner
duce higher energy density of 27.2 Wh/kg and 0.48 kW/kg power surface by electrostatic adsorption. In a three-electrode arrangement
density. Wu et al. [190] fabricated a Ti3C2@PDA/Ni2Co2S4 composite by using H2SO4 aqueous electrolyte, the prepared composite gives 366 F/g
hydrothermal method, polydopamine is an important member among specific capacitance at 2 mV/s scan rate greater than pure MXene (43 F/
polymer family act as a protective layer to provide good mechanical s) with a capacitive nature.3D printing for fabricating electrodes is a
stability and completeness to Ti3C2 in hydrothermal process but as a suitable method for assembling flexible supercapacitor devices. By using
super-hydrophobic nano-glue for stabilize NiCo2S4 nanoparticles over 3D printing, Yu et al. [195] prepared a NiCoP/Ti3C2 MXene hetero
Ti3C2⋅In a three-electrode system using KOH electrolyte it produces 495 structure ink printed on the polyethylene terephthalate substrate. This
F/g specific capacitance at 2 mV/s with better cyclic stability. Also, it robust open framework delivers 20 F/cm2 of areal capacitance. In the
retains 81.16 % capacitance retention after 3000 charge-discharge fabricated asymmetric device with 3D printed pattern as positive elec
cycles. trode and 3D printed activated carbon as negative electrode deliv
ered0.89 mWh/cm2 areal energy and 2mWh/cm3 of volumetric energy
6.6. MXene based other hybrids density in 2 M KOH electrolyte. Here they obtained the CV curve with a
combination of double layer and pseudo characteristics in agreement
By the use of efficient and convenient ion attraction method, Li et al. with the GCD curve.
[191] constructed a novel Bi2S3/Ti3C2Tx composite where the fallen leaf Zhang et al. [196] fabricated a flexible electrode with 2D Ti3C2
like Bi2S3 is planted over the Ti3C2Tx by the Ti atoms local repulsion and wrapped over 3D Ni-Fe oxide nanocube. The supercapacitor device is
by the functional groups –OH, –O, –F attraction to Bi3+.In a three- fabricated by coating the composite film into a polyethylene tere
electrode system with 1 M KOH aqueous electrolyte delivers 615 c/g phthalate flexible substrate with cellulose membrane soaked in PVA/
specific capacitance. Capacitive controlled and diffusion-controlled LiCl as separation between two film electrodes. The device delivers
process gives the improved supercapacitance. In the symmetric super 328.35 mF/cm2 specific areal capacitance at 0.2 mA/cm2 with 90.9 %
capacitor arrangement, it gives specific capacitance of 164 mAh/g at 16 capacitance retention after 10,000 cycles and good mechanical robust
A/g with 85 % of coulombic efficiency at 10 A/g. The durability with the ness. Under negative potential state, 2D Ti3C2 possess large capacitance
symmetric supercapacitor gives 91 % of capacitance retention after so it needs a suitable combination of another positive electrode for
1000 cycles. The electrochemical performance of the device is due to the symmetric configuration. So, the construction of MXene with another
specific van der Waals heterostructure. The device delivers 27.6 Wh/kg material facilitates the wide potential window in aqueous electrolyte. M.
higher energy density at 1944 W/kg higher power density and the de Boota and team [197] discovered the use of graphene oxide sheets hy
vice possesses good performance. At neutral pH, the quasi-solid-state bridized quinone-functionalized viologn molecules as pseudocapacitive
electrolyte avoids the flammability and corrosion properties with material and MXene as negative electrode. The prepared device estab
organic, acid/alkaline electrolytes. In order to overcome the issues lished a wide potential window of 1.5 V in 3 M H2SO4 solution, with 77
relating to the energy density of quasi solid-state device, Yang et al. % of capacitance retention from 10 to 1000 mV/s with ~20 Wh/kg
[192] developed flexible positively charged black phosphorus synthe energy density and 80 % capacitance retention after 10,000 charge-
sized by electrochemical exfoliation and it is then electrostatically discharge cycles. Chang et al. [198] fabricated a nacre-like composite
assembled to a negatively charged MXene collectively forming BP- film with Ti3C2Tx, cellulose nanofiber and sodium lignosulfonate by
MXene nanocomposite. Also, they fabricated a highly flexible quasi hydrothermal process. The prepared material shows good mechanical
solid state micro supercapacitor in symmetric configuration using a strength and conductivity. The symmetric supercapacitor device con
neutral electrolyte possess 28.17 mWh/cm3 volumetric energy density structed with this electrode material possesses a volumetric specific
at 0.043 W/cm3 with 68.7 % rate performance and 90.9 % cyclic sta capacitance of 748.96 F/cm3 with good energy density of 16.2 Wh/L and
bility after 40,000 cycles. Here the CV curve of prepared electrode excellent electrochemical cyclic stability. Li et al. [199] fabricated a
material possesses a quasi-rectangular shape with the GCD curve as an metal-ion hybrid microsupercapacitor with Zn-ion, where a Faradaic
isosceles triangle indicating the EDLC contribution of electrode in the cathode and capacitor type anode material is used in order to achieve
electrolyte due to the production of lamellar structure with introduction higher energy and power density. For this, they used Ti3C2Tx MXene as
of a porous network and heterostructure interfaces. Ti-O-P bonds capacitor type anode and V2O5 as battery type cathode. To finish the
improving the heterostructures interfacial atomic charge polarization structure of Zn-ion based microsupercapacitor ZnSO4 dissolved in
producing an efficient electron transfer, thereby the supercapacitive polyacrylamide (PAM) hydrogel is used as the electrolyte, which avoids
performance. Ramachandran and team [193] prepared Ti3C2/copper- the risk associated with the charge storage properties of other organic
Phthalocyanine (MPC) as a suitable electrode material for symmetric electrolytes with an introduction of long cyclic stability. They obtained a
supercapacitors. In a three-electrode setup, the electrode material gives specific capacitance of 129 mF/cm2 with a large energy density of 48.9
786.1 F/g specific capacitance. The fabricated symmetric supercapacitor μWh/cm2 at 673 μW/cm2. Their studies revealed that the metal ion-
delivers 8.84 Wh/kg energy density with 112.3 W/kg power density. based hybrid microsupercapacitor devices will provide good super
The device gives 92.3 % cyclic stability after 20,000 cycles with good capacitor performance with long cycle life.
coulombic efficiency. Here the rectangular shape of CV curves indicating 2D layered MXenes are possessing a demerit due to its oxidative
an ideal capacitive nature with efficient reversibility and stability and a instability and disintegration when it is in contact with water which
31
restricting its widespread applications in real-life. By understanding redox peaks in KOH and a pair of broad redox peak in H2SO4. In MgSO4,
this, Zhang et al. [200] fabricated an ultrafast supercapacitor with water there is no distinguishable peak is observed and the rate performance is
stability based on tartaric acid treated MXene/PEDOT: PSS conductive inefficient. The spacing occurred in MX layer is capable to accommodate
coating, which act as an electrode material. They followed an accurate the cations inserted/reinserted with 21 Å interlayer spacing. Abdoulaye
chemistry route for the assembling of the device, thereby they obtained Djire and team [207] prepared Mo2N by temperature programmed re
an areal capacitance of 1149 μF/cm2 and an 80◦ phase angle at 120 Hz. action with NH3. Due to the presence of mesopores and macropores the
With the introduction of stability by the fascinated performance of tar material has large pseudocapacitive value than double layer mechanism
taric acid they found that the fabricated ultrahigh rate filtering capacitor in H2SO4 electrolyte in H2O and D2O solvents. With in-situ small angle
holds better stability for aqueous systems. Shrabani De and team fabri neutron scattering they found that pseudocapacitive energy storage is
cated a symmetric and asymmetric supercapacitor based on Ti3C2Tx/ due to the H+ and e− ion insertion to the micropores producing a
polyindole nanocomposite by chemical oxidation method, where the reduction of Mo metal with good stability. They got 1500 F/g specific
polyindole is going to intercalate successfully to the MXene species capacitance in 1.2 V. By the selective etching of Al and Sc from MAX
thereby improving the supercapacitor performance of it. They obtained phase (Mo2/3Sc1/2)2AlC, Dr. J. Halim and team [208] prepared
a specific capacitance of 226.5 F/g at a current density of 2 A/g in Mo1.33CTz MXene. They obtained a good phase pure MXene without any
symmetric combination and a specific capacitance of 117 F/g in asym secondary phase. The prepared free-standing films and the electro
metric arrangement. Thereby they found that the preparation of a chemical performance were analyzed in a three-electrode cell. They
hybrid network based on MXene is a suitable method for the high- used gold foil as a current collector and Celgard 3501 immersed in 1 M
performance devices [201]. Currently, non-toxic MXene based device H2SO4 as a separator. They obtained 1308 F/cm3 volumetric capaci
got significant attention in bioelectronics. Among group IV transition tance with 98 % of capacitance retention and good cyclic stability. Their
metals, Tantalum possess interesting properties in comparison with results give a prominent pathway for the preparation of high quality
other MXenes, by understanding the properties of tantalum Rafieerad MXene supercapacitors with abundant elements such as Y vs Sc.
et al. [202] proposed a fluorine free exfoliation and functionalization of Chuanfang John Zhang and team [73] prepared a flexible, coplanar
tantalum carbide MAX phase for the preparation of Ta4C3Tx MXe architecture of microsupercapacitors by a cost-effective stamping
ne‑tantalum oxide (TTO) hybrid by using a modified fluorine free method. They prepared various stamp shapes which are coated with an
etching method. With the application of two-step acidic/alkaline treat ink of MXene printed and pressed to a flexible substrate and found that
ment they prepared this fluorine free tantalum based MXene. For the it’s possible to prepare the micro supercapacitor by this stamping
supercapacitor device fabricated from this hybrid, they got a specific strategy which is more cost effective than inkjet printing and direct 3D
capacitance of 447 F/cm3 with capacitance retention of 90 % after printing. The prepared micro supercapacitor (Ti3C2Tx) MXene exhibits
10,000 cycles and it shows that this biomaterial-based supercapacitor an areal capacitance of 61 mF/cm2 with long lifetime, large energy
has excellent stability for act as a futuristic energy device in a toxic free, density, power density, etc., in a box-shaped CV curve holds faster
environmentally friendly manner. 2D material-based electrodes are al current response in reversing the voltage indicating the capacitive
ways affected by the limitation in accessibility with the electrolytes, due charge storage nature. Flexible micro supercapacitors are prepared by
to the restacking of layers. By understanding this, Zhang et al. [203] this method. The supercapacitor device fabricated in inorganic electro
proposed a electrolyte mediated method for the integration of rGO/ lyte such as KOH and K2SO4 causes leakage and harmful atmosphere for
MXene-electrolyte composite films, where the electrolyte is intro human health. Aqueous electrolytes such as lithium, sodium, potassium
ducing a continuous ion transport channel between the composite films. salts are eco-friendly and produce large electrical conductivity, higher
Here the rGO-electrolyte composite film is fabricated by the synchro ion transport rate etc. and economic benefits. Based upon this factor, Xia
nous assembly of GO and MXene film on the Zn foil surface in electrolyte et al. [209] fabricated a symmetric supercapacitor based on sea water as
medium. With the highest accessibility of electrolyte ion, they obtained electrolyte which contains almost 0.46 M NaCl, to introduce a cheapest
a volumetric capacitance of 454.9 F/cm3 with energy density of 39.4 way of device fabrication. Herein, the CV curve maintains an approxi
Wh/L for the fabricated flexible supercapacitor. Their findings proposed mately rectangular shape with a non-symmetric sharpness in the GCD
a new route for the fabrication of dense structure films with 2D materials curves which is due to the incomplete redox reaction produced by the
for the flexible supercapacitor with higher volumetric capacitance active intermediate and reaction products which generated in the mes
value. By using a facile plasma treatment followed by thermal evapo opores and micropores. In the symmetric assembly of Ti3C2Tx/Ti3C2Tx
ration method, Abhinandan Patra and team fabricated a two-electrode configuration at 0.25 A/g, they obtained about 27.4 F/cm3 volumetric
symmetric supercapacitor device with passivated vertical graphene ar capacitance with 96 % capacitance retention after 5000 cycles. In order
rays as current collector. They obtained an areal capacitance of 199 mF/ to understand the phenomena behind the capacitance of Ti3C2Tx MXene
cm2 at 0.08 mA/cm2 with energy and power density of 13.57 μWh/cm2 in H2SO4 contain aqueous electrolytes is done by Hu et al. [210], by
and 31.07 μW/cm2 respectively and this high performance reveals that three different cations associated with in situ Raman spectroscopy. They
MXene/ vertical graphene arrays act as an efficient electrode material analyzed the electrochemical mechanism of Ti3C2Tx film by using
[204]. H2SO4, (NH4)2SO4 and MgSO4 electrolyte. They found that good voltage
Heteroatom doping is a suitable method for improving the specific dependent changes occurred in Raman bands which are associated with
capacitance of MXene because it makes a strong intercalation towards its Ti3C2Tx in the conditions that in H2SO4 electrolyte, electrodes are
layers thereby avoiding the aggregation and provides specific spacing. negatively charged. Fig. 22 shows the voltage dependent Raman bands
Nitrogen doped Ti2CTx, 900-N Ti2CTxis synthesized by Yoon et al. [205] when the electrode holds a negative charge in H2SO4 electrolyte. By
by sequential intercalation and carbon nitride decomposition with scanning of data in the range of 0 to − 0.4 V there is a prominent Raman
exfoliation and thermal annealing method. For the preparation of ni mode at 726 cm− 1. During backward scanning the peaks are shifted back
trogen doped Ti2CTx using cyanamide as a nitrogen source. With the in the reverse direction, at 530–770 cm− 1 range, there is a representative
synergistic interaction of 2D structure and N-doping the specific band points to the Lorentzian peak Fits (3) representing that as inter
capacitance is reduces to 327 ± 1 F/g at 1 A/g with 86.2 % capacitance calation goes further, the peak present at 726 cm− 1 is shifting towards
retention at 10 A/g, and good cyclic stability in 6 M KOH with a double the lower region of wave-number and strengthening it. In (NH4)2SO4
layer mechanism. Zhao et al. [206] fabricated Nb4C4Tx film from 413 and MgSO4electrolytes, the electrode shows EDLC behaviour due to the
MAX phases. The delaminated free-standing film have interlayer spacing counterion adsorption. Thus, hydronium ions are mobile in the three
of 177 nm and it exhibits higher volumetric capacitance in different electrolytes but it is more accommodated on the inner adsorption sites of
electrolytes such as 1075 F/cm3 in 1 M H2SO4, 687 F/cm3 in 1 M KOH Ti3C2Tx layers, thus this ion-exchange feature is contributing to higher
and 506 F/cm3 in 1 M MgSO4 at 5 mV/s. They obtained a one pair of charge storage mechanism in MXene confirmed by Raman.
32
7. Summary have to be encountered with proper strategic approach. The challenges

regarding MXenes in the field of energy storage is still a mystery to
In summary, 2D layered MXenes have got fascinating interest as an decipher. However, a few critical challenges have been listed out below.
electrode material by different energy groups due to its good conduc
tivity, wide potential window and layered nature for faster diffusion/ • Less availability of precursors
intercalation of electrolyte ions. Currently, there exists a rapid interest in • Higher cost of synthesis
MXene as an electrode material. Here in the present review, we gave an • Scalable route of synthesis
outline of various aspects of MXene as a supercapacitor, also its synthesis • Toxicity and environmental hazardless
methods and crystalline nature. There are two methods for the synthesis • Reduced rate of chemical and temperature stability
of MXenes: such as top-down and bottom-up methods. MXenes are • Less availability of proper theoretical simulations
usually synthesized by the etching method from its MAX phase using an
etchant commonly with HF or HCl-LiF. 2D MXene nanosheets have good 8. Conclusion and future perspectives
disposition to restack or aggregate during film electrode preparation
limiting the ion transportation formed in thin film and deteriorating the There are so many challenges are existed with MXene, but beyond all
electrolyte ion feasibility in the electrode. Thus, development of a good these, this new generation materials are still favorable for super
electrode material which having large open lamellar structure providing capacitor devices. By understanding the challenges and future goals we
spacious corridor place to introduce the storage of charge carrying ions can able to develop more MXene based supercapacitor devices in order
and shuttling producing an improvement in electrochemical perfor to avoid the current energy crisis and demerits with the already existing
mance. The construction of electrode structure involves the morpho energy storage devices. In a nutshell, this review explains the funda
logical transformation from planar MXene structure to a 3D mental features of MXenes such as its crystal structure and synthesis
interconnected network introducing a complex and a protected pathway methods. We introduced an outline of charge storage mechanism in
for ion diffusion and low density which shackles the performance of MXenes, factors affecting the supercapacitor mechanism in MXenes and
supercapacitor device at higher charging/discharging. Low dimensional various types of supercapacitor devices based on MXene. To avoid the
nanomaterials are considered to be as a feasible way for improving the restacking due to the presence of excess number of functional groups
performance of supercapacitors. From the reported papers it is found and to improve the supercapacitor performance of MXene based
that a simpler physical mixing doesn’t induce spacing between nano supercapacitor devices, we hereby proposed the details and capacitive
sheet layers, so it is failed to induce a faster kinetics and an efficient performance of MXene based hybrids with materials such as carbona
contact in electrolyte ions. The presence of excess number of terminal ceous species, TMOs, TMDs, etc. From this detailed investigation, we
groups such as oxygen and fluorine in the MXene sheets are going to found that the preparation of hybrid materials is to be considered as a
collapse the layered structure and the heaping of these layers from prominent approach to improve the supercapacitor performance of
lamellar structure thereby a reduction in supercapacitor performance. MXene based electrodes, but a detailed understanding of these materials
Thus, researchers are given their interest to avoid this demerit. MXene is necessary. However, other tactical strategies like phase engineering,
based composites are needed to be explored to avoid the demerits defect formation, introduction of magnetic field etc. can be fruitful to
occurred from the terminal groups. Higher cost of nanomaterials for enhance the charge storage performance of MXenes and primarily the
hybrid preparation is preventing its large-scale production, thus there cost optimization during fabrication is the vital thing to make accessible
exists a challenge in the construction of a cost-effective bridges between MXene based electrodes for supercapacitors in the global market. The
MXene sheets. Thereby, it is necessary to develop an eco-friendly and commercialization of these electrodes is only possible by successful
cost-effective route for the synthesis of MXenes. With respect to the standardization procedure, cost effectiveness compared to other avail
elemental compositions and functional group termination, about 100 able electrode in the market. More and more focus can be given in the
MXenes are predicted but only 25 types of MXenes are influencing the direction of fabrication of MXene based electrodes for real time device
properties such as mechanical, electrical, optical, etc. It is not possible to application so that aforementioned issues can be tackled head on. A lot
assure a good electrochemical performance from these synthesized of studies have been going on the microsupercapacitors, self-charging,
MXenes, currently existing MXenes are show good charge storage self-healing, photo powered supercapacitor etc. based on graphene
property only by the formation of hybrid/heterostructure. and other EDL materials. Likewise, MXene can be the ideal alternative
MXene act as an excellent electrode material for supercapacitor ap for graphene which will be the frontiers of allin optoelectronics world.
plications nevertheless its role in some other optoelectronics and bio Undoubtfully we can conclude that in the near future, MXene may
logical studies also have been proven to be phenomenal. The evolve as a superior robust electrode material for energy storage devices
electrocatalytic activity of MXene is also quite commendable as the for which a lot of areas still has to be investigated. Some major future
charge transfer characteristics are top notch and photocatalytic activity goals have been taken out from this current audit and furnished beneath.
is no less too. Some other field where MXene performed as the best of the
materials comprises of desalination and waste water treatment, tribo • Advanced scientific research for understanding surface chemistry,
electric and piezoelectric nanogenerators, corrosion studies, Sensors and tunability and interlayer structure for device fabrication
chemical noses etc. However, the objective of this review doesn’t • Preparation of more hybrid/heterostructure based on other materials
revolve around these studies. The detailed investigation regarding in MXene family more specifically non-Ti based MXene
MXenes in miscellaneous applications can be found elsewhere. • Fabrication of flexible, transparent and miniaturized MXene based
Therefore, in our present review we analyzed about the recent de supercapacitors.
velopments in the MXene based hybrid/heterostructure with Transition • Exploration of non-Ti based MXene
Metal Dichalcogenides, Carbonaceous materials, Transition Metal Ox • Engineering of defect states to control the properties
ides and Conducting Polymer. We found that the fabrication of a het • To understand the influence of stoichiometry, precursor’s
erostructure material with MXene is a suitable method for increase the morphology, concentration, etc., on the prepared MXenes
supercapacitor performance of MXenes. Thus, MXene based composites • Develop more micro supercapacitors and fabricate hybrid devices
are needed to be explored more in order to avoid the demerits occurred with solar cells, sensors, etc.
from the terminal groups. The major challenges and future perspectives • Study the device performance of MXene based materials in organic/
of MXene materials are given below: ionic electrolytes
Challenges: • Illustrate the influence of ions and molecules confined between
When it’s all said and done, there are some major challenges that MXene layers to the supercapacitor performance
33
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Journal of Energy Storage 55 (2022) 105765

Contents lists available at ScienceDirect

Journal of Energy Storage

MXene based hybrid materials for supercapacitors: Recent developments

1. Introduction based on electrochemical reactions, known as supercapacitors/electro

Fig. 1. Brief outline of the content of the review.

a deviation from the hexagonal arrangement and creating a Kagome-like Fig. 4.

Fig. 3. Top-down and bottom-up methods for the synthesis MXenes.

Fig. 4. Pictorial representation of etching processes of MXene from MAX phase.

Fig. 11. Properties of MXenes for supercapacitor applications.

(caption on next page)

Table 1 transportation. Then the heterostructure is shortening the trans

7. Summary have to be encountered with proper strategic approach. The challenges

You might also like

1 s2.0 S2352152X22017534 Main

Uploaded by

Document Information

Original Title

Copyright

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Share this document

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1 s2.0 S2352152X22017534 Main

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Copyright:

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Journal of Energy Storage 55 (2022) 105765

Contents lists available at ScienceDirect

Journal of Energy Storage

MXene based hybrid materials for supercapacitors: Recent developments

1. Introduction based on electrochemical reactions, known as supercapacitors/electro­

Fig. 1. Brief outline of the content of the review.

a deviation from the hexagonal arrangement and creating a Kagome-like Fig. 4.

Fig. 3. Top-down and bottom-up methods for the synthesis MXenes.

Fig. 4. Pictorial representation of etching processes of MXene from MAX phase.

Fig. 11. Properties of MXenes for supercapacitor applications.

(caption on next page)

Table 1 transportation. Then the heterostructure is shortening the trans­

7. Summary have to be encountered with proper strategic approach. The challenges

You might also like

1. Introduction based on electrochemical reactions, known as supercapacitors/electro

Table 1 transportation. Then the heterostructure is shortening the trans