Wa0009.

Materials Reports: Energy 2 (2022) 100080
Contents lists available at ScienceDirect
Materials Reports: Energy

journal homepage: www.keaipublishing.com/en/journals/materials-reports-energy
Review
MXenes with applications in supercapacitors and secondary batteries: A

comprehensive review
Xueqin Xu a, Li Yang a, b, Wei Zheng b, Heng Zhang a, Fushuo Wu a, Zhihua Tian a, Peigen Zhang a, *,
ZhengMing Sun a, **
a
Jiangsu Key Laboratory of Advanced Metallic Materials, School of Materials Science and Engineering, Southeast University, Nanjing, 211189, PR China
b
Department of Physics, Chemistry and Biology (IFM), Link€oping University, Link€oping, 58183, Sweden
A R T I C L E I N F O A B S T R A C T
Keywords: Two-dimensional (2D) materials have received tremendous attention because they possess a set of merits not
2D materials available in bulk materials, such as large specific surface area, low energy barrier for electron transportation and
MXenes short ion diffusion path. These advantages are desirable especially for the electrodes in electrochemical energy
MAX phases
storage devices. MXenes, first synthesized in 2011 by etching their MAX phase precursors, have plural reasons to
Batteries
represent a new family of 2D materials. Their rich diversity in structure and composition together with the un-
Supercapacitors
common combination of good electrical conductivity and hydrophilicity makes themselves outstand in the whole
2D materials world. Based on these advantages, MXenes hold great promise for various technologically important
applications, particularly in developing new energy storage techniques for advanced smart systems, such as
portable and flexible electronics. There have been remarkable research achievements in the synthesis and
application of MXene-based materials. While new synthesis routes being continuously reported, MXenes with new
composition and novel structure have also been routinely discovered, which will undoubtedly help understand
the fundamental properties and expand the application scope of MXenes. As for their energy storage-related
applications, to cope with the intrinsic weakness of MXenes, many endeavors have been made by doping,
structure-tuning and compositing with hybrid ingredients. In this review, the current status of MXenes synthesis
and up-to-date progress of their applications in supercapacitors, metal-ion batteries and lithium sulfur batteries
are summarized and discussed, and the typical work on the application of MXenes for the aforementioned three
categories is respectively tabulated for reference and comparison.
1. Introduction materials, such as large specific surface area due to their atomic thick-
ness, low energy barrier for electron transportation because of their
Two-dimensional (2D) materials are single-/few-layer crystals, and crystalline nature and short ion diffusion path generated by their layered
usually have fascinating properties, compared with their 3D bulk coun- structure. These merits just correspond to the requirements and the
terparts, because of dimension dependence of the materials properties.1 developing trend of electrodes for electrochemical energy storage.6,7
Therefore, 2D materials have been extensively studied, which was Therefore, great expectations have been placed on the 2D materials to
further pushed in 2010 as the Noble prize in physics was awarded for cope with the current energy issues and the ever-increasing demands for
groundbreaking experiments regarding the first 2D material graphene.2–5 advanced energy storage devices.8 Graphene is undoubtedly the most
Apparently, 2D materials possess a host of merits not available in bulk studied 2D material for energy application,3,9 and, in fact, most of 2D
* Corresponding author.
** Corresponding author.
E-mail addresses: zhpeigen@seu.edu.cn (P. Zhang), zmsun@seu.edu.cn (Z. Sun).
Production and Hosting by Elsevier on behalf of KeAi
https://doi.org/10.1016/j.matre.2022.100080
Received 5 November 2021; Received in revised form 13 January 2022; Accepted 17 January 2022
Available online 2 February 2022
2666-9358/© 2022 Chongqing Xixin Tianyuan Data & Information Co., Ltd. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an
open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
X. Xu et al. Materials Reports: Energy 2 (2022) 100080
Fig. 1. Different types of MXenes. Reproduced with permission from Ref. 75.
materials have been investigated on energy applications,1 such as tran- normally, n ¼ 1–3, and correspondingly referred to as 211, 312 or 413
sition metal oxides (e.g., iron oxide,10 and NiO11), dichalcogenides (e.g., phase, respectively.) are a vast group of layered compounds, currently
MoS2,12 and WS213), hexagonal BN,14 hydroxides,11 organics,15–17 and having more than 130 members and many more with tunable composi-
elemental 2D nanosheets (referred to as Xene,18,19 X ¼ Si,20 Ge,21 P,22 tions if we consider the solid solutions for M/A/X sites, such as (Ti0.5Nb0.5)
and so forth). The hope on developing advanced energy storage materials AlC,69 V2(Ga1-xAlx)C (0.43 < x < 0.6),70 and Ti3Al(C0.5N0.5)2.71 The
was sufficiently lighted up by all the efforts made on these 2D materials. MXenes family inherits the big size of MAX phase family, and has exper-
A group of compounds consisting of few-atom-thick layers of transi- imentally found ~30 members with different compositions (more theo-
tion metal carbides, nitrides, or carbonitrides, collectively denoted as retically predicted).26,27,29,67,72 As seen in Fig. 1, the big family has a
MXenes (to emphasize their graphene-like morphology), have multiple general formula: Mnþ1XnTx, where M, X and the number n have the same
reasons to represent a new family of 2D materials.23–27 They not only meanings as those in their parent MAX phases, and Tx denotes surface
share the common fascinating properties of 2D materials, but also have terminations (usually a combination of various types, for example, –OH,
more desirable characteristics, such as rich chemical composition possi- –O, –F, and new terminations being bonded, for example, –Cl73) formed in
bilities,25 tunable surface chemistry,28 unusual combination of metallic the synthesis and post-synthesis processing phases.25 Recently, MXenes
conductivity and hydrophilicity and some other intriguing elec- having a formula of M1.33XTz were synthesized from in-plane ordered MAX
tronic,29,30 magnetic,31 optical30,32 and thermoelectric behaviors.33 As phase solid solutions.74
2D materials are finding their way into a huge number of applications, Benefitting from the pioneering work accumulated for several couples
MXenes, due to their versatile chemistry and the rich room for surface of years on the research and development of 2D materials (notably, gra-
modification, has found a significant place in diverse technological phene and MoS2), and also because of their outstanding potential and
applications,4,6,25,27,34,35 and can be tuned for a much broader spectrum upside, the MXene-related research has exploded. This explosion leads to a
of applications, including energy storage,25,27,29,36–46 catalysis,47–50 continuously growing MXenes family, discovers more fundamental science
sensors,51–56 electromagnetic interference (EMI) shielding,57,58 envi- on their chemistry/physics, and has much more applications demonstrated
ronment management,59–61 polymer-based composites,62 lubrica- or proposed.26,67 Among the numerous applications of MXenes, fabrication
tion,63,64 antibiosis,5,65 to name a few. Among these various vigorously of MXene-based various electrochemical energy storage systems is one of
developing areas, MXenes as energy storage materials have received the top-ranking areas and vigorously developing. New work and results
increasing attentions since their intrinsic structure and properties impart appear every day in large numbers. In this review, trying to provide an
them particular advantages of being electrode materials in electro- updated map for the readers engaged in developing high-performance
chemical energy storage devices.4,27,28,34,66,67 Actually, as Ti3C2Tx was MXene-based energy storage systems, we summarize and discuss the
first produced, applications in Li-ion batteries and supercapacitors were up-to-date progress of the synthesis of MXenes as well as their MAX pre-
immediately suggested according to its good conductivity and suitable cursors and their applications in selected areas. Especially, the typical
interlayer space.24 In the past decade, since the discovery of its first works in supercapacitors and secondary batteries are summarized and
member of Ti3C2Tx in 2011 at Drexel, MXenes have been becoming one listed in tables for convenient reference and comparison.
of the most promising electrode materials.24
MXenes are synthesized by selectively etching their corresponding 2. Synthesis, structure and properties
parent MAX phases, for example, Ti3C2Tx (Tx, such as –F, –O, and/or –OH)
from Ti3AlC2.24,25,68 MAX phases (short for their general formula: Preparation methods for 2D materials can generally fall into two
Mnþ1AXn; M: early transition metal; A: group A elements; X: C and/or N; categories: top-down and bottom-up approaches. As shown in Fig. 2.
2
Fig. 2. Synthesis of MXenes. (a) Molten salts etching, (b) Modified fluoride-based acid etching, (c) Chemical vapor deposition, (d) Fluoride-free etching. Reproduced
with permission from (a) Ref. 82, (b) Ref. 83, (c) Ref. 84, (d) Ref. 85.
Most of MXenes in the open literature are currently synthesized via a top- near-close-packed M layers and the group-A element layers with the
down protocol, viz., the chemical etching approach directly or indirectly former layers’ octahedral sites filled by X atoms (forming M6X octahe-
involving HF,26,67 although bottom-up preparation strategies have been dral),69,86 and different value of n modifies simply the number of M6X
continuously reported, such as by chemical vapor deposition (CVD),76–79 layers between each A-element layer. Most of the unusual properties and
salt-template,80 and laser deposition.81 These new bottom-up routes behaviors of MAX phases can be traceable to this structure and the
significantly advance the research on MXenes, since they can grow high accompanying characteristic of chemical bonds, such as being able to
quality MXenes with large lateral size, few defects, and chemical com- etch selectively,27 and the ability to reconcile the advantageous proper-
positions currently unattained by etching.26,27 It is worthy of noting that ties of metallic and ceramic materials which are incompatible
single layer MXenes have not yet grown via these strategies, albeit the elsewhere.86
as-grown films can be ultrathin (a few nanometer thick).77 These MAX phases are receiving much more attention from a broader
bottom-up strategies should be further explored and are expected to grow community as they are not only finding their way to practical
MXene monolayers to facilitate the investigation on their intrinsic applications,69,86,87,90–92 but also playing the critical role in the big game
properties and extend their applications to more sophisticated devices. MXenes launched.26,67,93,94 The upsurge of interest in this area have
As for the most adopted top-down MXenes preparation method, extend the territory of M and A elements in the periodic table for MAX
different from that for the preparation of most other kinds of 2D materials phases.88 As a result, new MAX phases unprecedentedly containing Zn,73
where Van de Waals’ force (secondary bond) is manipulated (e.g., me- Au/Ir,95 Cu,96 Mn,97 Bi,98 etc. come to light, enriching the chemical di-
chanical exfoliation of graphite),1 MXenes are produced by selectively versity both for M and A sites. Currently, most of parent MAX phases for
etching the primary bonds between M and A atoms in their parent MAX MXenes are Al-containing, and as more new members of MAX phases are
phases and it follows by chemical exfoliation (to obtain delaminated synthesized, it is expected to break this limitation. Also, some interesting
MXene flakes).4,26,29 Consequently, MXenes are the first 2D materials MAX phases with chemical ordering (out-of-plane order and in-plane
produced by disrupting primary bonds, and in that sense, MXenes also order, so-called o-MAX and i-MAX, respectively) were reported
deserve a title as a new family of 2D materials. recently, which are different from the random solid solutions of MAX
The merits such as high yield, efficiency, ease of scalability, and phase found in early years.72,99,100 For the o-MAX phases, a single (such
aqueous solution-processability are found in the top-down preparation as Mo2TiAlC2),101 or double (such as Mo2Ti2AlC3),102 layer of one kind of
route of MXenes, and they are vital to the possibly practical applications. M element is sandwiched between layers of a second M element; and for
In view of this, this section focuses on the etching preparation method, the i-MAX phases, it means the in-plan order of two kinds of M elements,
and the typical literature on MAX phase precursors, etching protocols, such as (Mo2/3Sc1/3)2AlC,74 (Mo2/3Y1/3)2AlC and (V2/3Zr1/3)2AlC.103
multilayer and delaminated MXenes and MXene films are summarized These new developments have been reshaping the family of the layered
and discussed. solids, rendering new opportunity for MAX phases themselves, and this
opportunity might be also transmitted to their derivative MXenes. This
2.1. MAX phase precursors trend is demonstrated that the term “ternary” is not emphasized any
more as MAX phases were referred to and discussed a couple of years
As noted above, it is inevitable to understand MAX phases before ago,86,104–107 because they may contain four or even more elements and
coming to MXenes. There are well-recognized existing reviews and offer many more fascinating structural novelties.
monograph to provide comprehensive knowledge on MAX phases and It is the low bonding strength of M-A and large ratios between the
their history.69,86–89 MAX phases can be viewed as a class of thermody- bonding strengths of M-X and M-A that make the MXenes possible out of
namically stable nano-laminates, as it was called before the term MAX MAX phases.108 Therefore, in addition to MAX phases, several other
(Mnþ1AXn) phase was coined by Barsoum in 2000.87 They share a unique layered compounds which have similar bonding characteristics with but
crystal structure which is constructed by the alternating stacking of the are structurally different from MAX phases were also successfully etched
3
Fig. 3. Illustration of the relationship of MAX and MXenes, depicting the synthesis process of MXenes using HF as the etchant. Reproduced with permission
from Ref. 26.
to obtain their 2D MXene counterparts. Mo2C was synthesized from a choice of etchant is very critical to successfully carry out the selective
precursor of Mo2Ga2C,109 in which Mo6C layers are separated by two Ga etching. The vast majority of the ~30 different MXenes currently ob-
layers instead of one as in MAX phases. Hence, it does not belong to the tained via wet chemical route are realized by etching the Al layers from
family of MAX phases. Another group of layered structures capable of their respective Al-containing MAX phase precursors27; but, not all
giving birth to MXenes has formulae of (MC)nAl3C2 and (MC)n(Al,Si)4C3 Al-containing MAX phases are successfully etched, and MAX phases
(M: Zr or Hf, and n ¼ 1, 2 or 3),110 and, for example, Zr3C2Tz111 and without Al have been seldom reported to successfully etched to MXenes,
Hf3C2Tz112 were demonstrated by selective etching of the layer of Al3C3 with an exception of Ti3SiC2, etched in a harsher HF/H2O2-contained
and (Al,Si)4C4 in Zr3Al3C5 and Hf3Al4C6, respectively. solution than just HF for Ti3AlC2 etc.113 In 2019, Li et al. reported the
To conclude, the ever-increasing diversity of MXene composition and successful synthesis and etching Zn-containing MAX phases, which is a
structure would definitely continue as MAX phases (and beyond) expand, new route to obtain MXenes although the starting point was still the
though etching different MAX phase does not necessarily bring about Al-containing MAX phases.73
MXenes with various compositions (e.g. etching both Ti3SiC2113 and Currently, the etching systems for Al-containing MAX phases are
Ti3AlC224 resulting in Ti3C2Tx). At present, the etching approach is becoming diverse, and a host of agents/conditions are used solo or
mostly restricted to the Al-containing MAX phases, which limits the multiply, including acid (basically, HF),24,118 alkali,119–121 salts,122 Lewis
potentially huge diversity space of MAX phases. As more MAX phases are acid,73 hydrothermal effect,123 electrochemical etching.118,124 And usu-
experimentally obtained, the corresponding MXenes would be expected ally, temperature is increased to promote the etching in a
if the suitable etching methods were found. Therefore, the suitable solution.113,120,125,126 Figs. 2 and 3 are from an up-to-date review
etching methods should be explored continuously to fully understand the article26 on the synthesis of MXenes by Verger and Barsoum et al. for the
etching process, and thus make the most of the diversity of MAX phases. excellent summary of the precursors, etching conditions and the high-
lights for virtually all of the MXenes preparation methods ever known. It
2.2. Etching MAX towards MXenes is important to note that various synthesis methods can significantly
influence the attributes of the resulting MXenes, including the yield,
The unique combination of the chemical bonds in MAX phases – morphology, structure, defects, surface terminations, delamination effi-
exceptionally strong MX bonds (mainly covalent and ionic) and the ciency when exfoliated to delaminated MXene and so on.
relatively week MA bonds (metallic) – makes the selectively etching Therefore, different synthesis route should be chosen properly
possible, deconstructing the relatively weak interlayer bonds and depending on the specific application/research purposes,127,128 and to
simultaneously keeping the in-plane bonds between M and X reserved as date, most research in literature adopts the synthesis protocols involving
pristine as possible. However, this selectivity cannot involuntarily HF (directly added or in-situ formed) thanks to the good controllability
happen for a given MAX-etchant system, and the success of selectively and ease of implement. However, it is clearly known that the HF etchant
etching MAX into MXenes strongly depend on the chemistry and the is a hazardous substance with the potential for bringing about systemic
crystal structure of the MAX phase precursor. toxicity to human body; in addition, the attachment of fluorine element
Early attempts to etch MAX phase started long before the discovery of on MXenes would influence their properties as well as limit the appli-
MXenes, such as etching Ti3SiC2 etc. to carbide-derived carbons using cation scope of MXenes. For example, theoretical and experimental in-
chlorine as early as in 2003,114,115 the dissolution of Si from the Ti3SiC2 vestigations indicate that –F groups markedly influence the properties of
into the molten aluminum,116 and others.117 However, none of the at- MXenes.46 Ti and C are benign, and thus MXenes would be suitable for a
tempts resulted in 2D structures before Ti3C2Tx was born by etching its variety of biological applications (for example, photothermal agents
parent Ti3AlC2 at room temperature in a solution of 50% concentrated against tumor,119,129 bioimaging130), but the –F termination would be
hydrofluoric acid.24 And therefore, the match between the MAX phase problematic with living bodies. In consequence, green routes suitable for
(both chemical composition and crystalline structure count) and the large volume production of MXene are necessary, and developing
4
Fig. 4. Methods of fabrication of MXene-based films: (a) rolling, (b) V014, Macmillan. (c) spin coating, (d) electrophoretic deposition (EPD), (e) spraying, (f) chemical
vapor deposition (CVD). Reproduced with permission from (a) Ref. 29, (b) Ref. 150, (c) Ref. 125, (d) Ref. 151, (e) Ref. 32, (f) Ref. 152.
fluoride-free synthesis routes have been an important endeavor branch of parameters to control. A higher etching temperature and longer reaction
this research area.118,126,131,132 Nevertheless, the toxicity of HF does not time can result in high concentration of defects and reduce the yield of
eclipse the etching methods using HF (the most efficient way to syn- the delaminated MXenes in the following exfoliation process.46,125,134
thesizing MXenes in large scale), and this toxicity issue would be prac-
tically resolved since the fluorine industry has been a mature industrial 2.4. Delaminated MXenes
sector for several decades.
Delaminated MXenes (often written as d-MXenes in literature) are
2.3. Multi-layered MXenes resulted from exfoliating m-MXenes, and the relationship of m-MXene
and D-MXene is just like graphite and graphene. At present, the major
As stated above, due to the relative simplicity and good controllability approaches to prepare d-MXenes are usually as follow. Firstly, weaken
of the etching systems involving HF, they are the most commonly the interlayer bonding in m-MXenes by increasing the interlayer spacing
adopted thus far.46 Etching the starting MAX phase in a hydrofluoric via appropriate intercalation, and then exfoliate the intercalated m-
solution, the A-atom layers (basically aluminum) in the MAX phase MXenes into d-MXenes, as shown in Fig. 3 (single layer MXene), via ul-
precursors are removed and are substituted by terminations, resulting in trasonic or other kinds of agitation.46
multilayered MXenes (commonly referred to as m-MXenes or ML MXenes For many of layered materials (e.g., clays and graphite), intercalation
in literature).29,46 is a well-established phenomenon.135 The intercalation also happens to
As shown in Fig. 3, MXenes obtained by etching in a HF-containing the layered m-MXenes, and a host of species such as polar molecules and
solution usually have an accordion-like morphology.24,26,38 The yield metal ions, can be used to intercalate m-MXenes. Frequently-used
of MXenes after etching is commonly above 50% (imprecise determina- intercalation agents include dimethyl sulfoxide (DMSO), dime-
tion due to the complexity of the functional groups and intercalated thylformamide (DMF), hydrazine (HM), urea, ammonia and
species).25,125 A number of attributes of m-MXenes would be influenced others.46,125,136,137 In addition, alkalis,138,139 organic molecules,140 aryl
by the etching conditions, most importantly, type of etchant, concen- diazonium salts,141 and cations (Liþ, Naþ, Kþ, Mg2þ, Al3þ, etc.) in
tration, reaction temperature and time, particle size of MAX precursors.46 aqueous salt solutions142 can also intercalate into m-MXenes, leading to
For example, milder etching systems such as the mixture of LiF and HCl the increase of their interlayer spacing.
result in MXenes with larger lateral size and less nano-sized defects as The preparation process of d-MXenes can be streamlined by simul-
commonly observed in MXenes etched by HF solution125; Ti3C2(OH)2 taneously realizing the etching and intercalation processes. And the
MXenes etched by NaOH (with small amount of water) are streamlined two-step routes also bring about other advantages, such as
large-lateral-sized nanoflakes, and easy to delaminate and restack120; higher yield of d-MXenes and less defects. Therefore, the two-step routes
surface groups of –F cannot be avoided by any methods involving HF or prevail.143 Alhabeb et al. gave the guidelines for synthesis and processing
villiaumite26,46; some alkaline etching systems only etch the aluminum of the most widely studied and used Ti3C2Tx MXene, describing the
atoms in shallow surface of MAX phases133; defects in MXenes often experimental methods, and also explaining effects of synthesis parame-
depend on the HF concentration in the used etching system.134 To obtain ters on the quality and size of Ti3C2Tx.144
high quality MXenes, etching time and temperature are also critical
5
Table 1
Preparation methods for MXene films and their applications.
Materials Methods Applications References
153–155
Ti3C2Tx Vacuum-assisted Membrane: gas
filtration separation, water
purification
156,149
Ti3C2Tx Vacuum-assisted Thin film, supercapacitor
filtration
157
Ti3C2Tx Spray coating Transparent thin film:
optoelectronic properties
146
Ti3C2Tx Spincasting Thin film: optoelectronic
properties
158
Ti2CTx Dip coating Thin film: transparent
conductive electrode
159
Nafion- Casting Filter
Ti3C2Tx
160
Ti3C2Tx Electrospray Thin film: optoelectronic
properties
161
Ti2CTx Spincasting Thin film: optoelectronic
properties
162
Ti3C2Tx Spin coating Flexible film,
supercapacitor
163
Ti3C2Tx Self-assemble Flexible film,
supercapacitor
164
Hollow Vacuum-assisted Thin film, SIBs
MXene filtration
spheres Fig. 5. Crystal structure of MAX phases and corresponding MXenes after
140
Ti3C2Tx/ Vacuum-assisted Flexible film, selectively etching. Reproduced with permission from Ref.180.
PDDA filtration supercapacitor
165
Ti3C2Tx/ Vacuum-assisted Flexible film,
PEDOT:PSS filtration supercapacitor outlines the frequently used methods for preparing MXene films and the
166
Ti3C2Tx/PAN/ Vacuum-assisted Film filter corresponding applications.
PEI filtration
167
Ti3C2Tx/PPy Vacuum-assisted Flexible film,
filtration supercapacitor 2.6. Structure and selected properties of MXenes
168
Ti3C2Tx/PAM Casting Flexible film
169
Ti3C2Tx/ Electrospray Flexible film, transport
Graphene properties As illustrated in Fig. 5, MXenes have a similar hexagonal crystal
Ti3C2Tx/ Vacuum-assisted Flexible film, all-solid- 170 structure to their MAX phase precursors. The MX layer is directly
Graphene filtration state supercapacitor inherited from MAX phase, and thus the rich diversity of MAX phase
171
Ti3C2Tx/rGO Vacuum-assisted Flexible film, LIBs offers large room to tune the structure and properties of MXenes.177 It is
filtration
Ti3C2Tx/CNT Vacuum-assisted Flexible film, LIBs 172 difficult to determine the precise structure of MXenes because of the
filtration inevitable terminations attached to their surface as being etched. In-
173
Ti3C2Tx/CNT Self-assembly process Flexible film, SIBs vestigations on the structure of MXenes are often conducted by theo-
and vacuum-assisted retical computation, since non-terminated MXenes have not synthesized
filtration
174 yet so far. In some first-principles studies, although surface terminations
Ti3C2Tx/ Vacuum-assisted Flexible film,
MnO2 filtration supercapacitor have been considered, limitations still remain, such as assuming the
MnOx/ Vacuum-assisted Flexible film, 175 uniform distribution of single type of terminations, resulting in some
Ti3C2Tx filtration supercapacitor discrepancies between the predictions based on the calculations and
176
Ti3C2Tx/SA Vacuum-assisted Electromagnetic experimental measurements.46,178,179
filtration interference shielding
Terminations on MXene surfaces render them hydrophilicity while
not apparently changing their conductivity. This unique merit brings
many advantages for MXenes over many other 2D materials. A compre-
2.5. MXene films hensive discussion on the surface chemistry of MXenes can be found in a
review by Yu et al.28 MXenes are quite sensitive to oxygen (especially in
MXene films can be made from d-MXenes. A set of excellent proper- elevated temperatures) due to the exposed metal atoms on their surfaces.
ties such as flexibility, hydrophilicity, conductivity and good mechanical For example, Li et al. reported Ti3C2Tx would be oxidized to TiO2 at
strength make the films promising electrodes for energy storage devices, 200 C in an oxidizing atmosphere,137 and Ying et al. found delaminated
such as supercapacitors and secondary batteries.125,145 The free-standing Ti3C2Tx transformed completely into rutile-TiO2 after three months
MXene films can get rid of binders, current collectors and conductive storage in water.181 Therefore, appropriate measures should be taken to
agents, and thus offer higher specific capacitance/capacity. In addition, avoid oxidation of MXenes when stored. On the other hand, however, the
the films also have potential applications for transparent electrodes, oxidation of MXenes can be also harnessed to obtain composites with
flexible screen, transistors and many other areas.27 much improved performance for some applications. For example,
Various methods have been developed to fabricate MXene films, such TiO2/carbon composite with excellent electrochemical performance was
as vacuum-assisted filtration, spray coating, painting, spin coating and fabricated by partially oxidizing Ti3C2Tx at 1150 C,182 and this oxidizing
rolling,125,144,146 as shown in Fig. 4. The MXene films fabricated by route can be further controlled to tune the structure of the resultant
various methods may have different properties, and thus for different materials,183 which is a promising research topic on MXenes. Mechanical
purposes, different methods should be appropriately chosen and properties of MXenes are usually investigated by first-principles calcu-
employed. For example, micro-thick transparent films can be made by lations. Kurtoglu et al. calculated the electronic and elastic properties of a
spin casting, and used for optical and electronic components147; series of MXenes, such as Ti2CTx, Ti3C2Tx, Ta2CTx, and obtained similar
vacuum-assisted filtration is suitable for preparing MXene films used as results to the MAX phases. These MXenes are metallic and possess high
electrodes for supercapacitors and secondary batteries.148,149 Table 1 elastic moduli within their basal planes.184
6
Fig. 6. Map of the keywords of the highly cited papers about MXene-based energy storage materials (constructed using VOSviewer, a free bibliometric anal-
ysis software).
To summarize, MXenes have tunable structure and chemical com- transition metal atoms renders MXenes good electrical conductivity and
positions, and new properties would be explored with the fast develop- high pseudocapacitance, and after removing A-atom layers in MAX phase
ment of newly synthesized routes. High performance energy storage precursors, the increased space between MX layers in MXenes can
materials as well as other advanced components would be enabled by accommodate a number of ions (such as Liþ/Naþ/Kþ). Therefore,
realizing such advantages of MXenes. MXene-based materials are born to be electrode materials, and actually
they are very promising for a series of energy storage applications.
3. MXene-based materials for energy storage Numerous research works about the MXenes used as energy storage
materials have been published, and the landscape of this area can be
With the rich variety of structures and compositions, MXenes visualized using VOSviewer, a freely available software tool for con-
outstand in the 2D materials world.185 Containing carbon layers and structing bibliometric networks in terms of researchers, keywords, and
Fig. 7. Schematic of different strategies to improve the electrochemical performance of MXenes. (a) MXenes doped with N by heat treatment. (b) Molten-salt-assisted
electrochemical etching method to synthesize fluorine-free Ti3C2Cl2. (c) Ti3C2–Cu/Co hybrids via molten salt etching. (d) 3D macroporous film by sacrificial template
method. (e) Nanoporous film by sacrificial template method. (f) Porous MXene nanosheet. (g) Composting MXenes with rGO. (h) Composting MXenes with MnO2. (i)
Composting MXenes with PPy. Reproduced with permission from (a) Ref. 202, (b) Ref. 206, (c) Ref. 209, (d) Ref. 164, (e) Ref. 207, (f) Ref. 172, (g) Ref. 210, (h)
Ref. 174, (i) Ref. 211.
7
many other aspects of interest. We were analyzed ~1500 highly cited was obtained at 5 A g1 and no significant degradation was observed
papers (published since 2011) and mapped their keywords to spot the after 10,000 cycles. A molten-salt-assisted electrochemical etching
focuses and the major links of this area, as shown in Fig. 6. As expected, method has been presented by Shen and his colleagues.206 Using elec-
the applications of MXenes in energy storage field focus on super- trons as reaction agents, cathode reduction and anode etching were
capacitors, metal ion batteries, and lithium sulfur batteries, benefited spatially isolated, the surface terminations were in situ modified from –Cl
from its significant features, such as 2D structure, good conductivity and to –O and/or –S, which considerably shortens the modification steps and
high specific surface area. enriches the variety of surface terminations. The obtained –O-terminated
Indicated by the primary nodes in the map (Fig. 6) is that Ti3C2Tx is Ti3C2Tx are excellent electrode materials for supercapacitors, exhibiting
the most frequently used MXene member for energy storage material capacitances of 225 F g1 at 1.0 A g1, good rate performance (91.1% at
fabrication, and supercapacitors, lithium-ion batteries (LIBs), sodium-ion 10 A g1), and excellent capacitance retention (100% after 10,000
batteries (SIBs), and lithium–sulfur batteries (LSBs) are the major devices charge/discharge cycles at 10 A g1).
where the MXenes are employed. To enhance the electrochemical per- The microstructure of MXenes can be also modified to increase the
formance (e.g., capacitance, capacity, energy density, cycling stability) of active sites and specific surface areas, which in turn improve the elec-
the devices, intense attention has been paid to the properties (e.g., trochemical performance. For example, interconnected nanopores
electrical conductivity, surface termination, restacking) of the MXene- (3–5 nm) were introduced into MXenes by using template of Fe(OH)3
based electrodes. In the following sections, we summarize and discuss nanoparticles. The nanopores formed channels promoting ion transport
the representative words about MXene applications in supercapacitors at no obvious cost of the ultrahigh density of MXenes and conductivity.
and secondary batteries. These combined merits led to an attractive volumetric capacitance
(1142 F cm3 at 0.5 A g1), good rate capability (828 F cm3 at
3.1. Applications in supercapacitors 20 A g1), high volumetric capacitance of 749 F cm3 and good flexibility
even at a high mass loading of 11.2 mg cm2.207 Organics were also used
Electrochemical supercapacitors (ES) are among the ideal solutions to assist to alter the microstructure of MXenes. 3D macroporous MXene
for powering portable digital products and electric vehicles thanks to the film was fabricated via a sacrificial organic template approach, which
high power density, fast recharge ability, long cycle-life, environment- delivered an excellent rate performance of up to 210 F g1 at an ultrahigh
friendliness, etc.186 scan rate (10 V s1).156 Besides, Zhao et al.208 fabricated the flexible
MXene-based electrodes, especially the free-standing films made from MXene films on Zn surface by the synchronous reduction and
MXenes hold great promise for supercapacitors and flexible electro- self-assembly strategy. The final product demonstrates high electrical
nics.187–192 In KOH electrolyte, binder-free Ti3C2Tx paper can achieve a conductivity, large specific surface area, and excellent mechanical
volumetric capacitance of 442 F cm3 at 2 mV s1 and exhibit almost no properties so that displays excellent and stable electrochemical perfor-
degradation after 10,000 cycles at 1 A g1.142 In H2SO4 electrolyte, mance even under various bending states.
Ti3C2Tx clay electrodes have a volumetric capacitance of up to To mitigate restacking of MXene nanosheets, interlayer spacers, such
900 F cm3 at 2 mV s1 and do not degrade after 10,000 cycles at as carbon nanotubes (CNTs),173,212 reduced oxide graphene
10 A g1.125 MXene hydrogels designed by Lukatskaya et al. were able to (rGO),188,210,213 Black phosphorus (BP),214 metal oxides,174 and polymer
deliver volumetric capacitance of ~1500 F cm3.156 These impressive molecules,167,211,215,216 have been introduced between the MXene
results open a new door for the application and prospect of MXenes in nanosheets, constructing hybrid electrodes, which can also take advan-
supercapacitors. However, to commercialize the MXene electrodes in tage of the different components to enhance the electrochemical per-
ECs, further improvement is needed. So far, as categorized in Fig. 7, the formance.210 For example, electrodes fabricated by compositing
efforts associated with improving the MXene-based SC electrodes fall into d-Ti3C2Tx and CNTs offered a capacitance of 393 F cm3 at 5 mV s1,
the following categories: tuning the chemical composition of MXenes, with higher cycling stability than that of metal oxides.217 With the
modifying the microstructure of MXenes, and compositing MXenes with assistance of an in situ sacrificial metallic zinc template, 3D porous
heterogeneous materials. oxidation-resistant (PMG) composite was prepared, the composite dis-
Heteroatom doping is a common strategy to improve the electro- played remarkable electrochemical supercapacitive performances, such
chemical performance of electrode materials, such as activated carbon, as unparalleled specific capacitance of 393 F g1 and spectacular cycling
graphene.193–200 Boron (B), Nitrogen (N), Phosphorus (P) and Sulfur (S) stability with no obvious degradation after 30,000 cycles.218 The pseu-
have been successfully introduced into the MXene nanosheets to improve docapacitive behavior of transition metal oxides gives them additional
their conductivity, hydrophilicity, and pseudocapacitance. N-doped advantages when used to composite with MXenes to prepare high per-
m-Ti3C2Tx was prepared by Tang et al. via hydrothermal reaction, and its formance electrode materials for SCs. For example, TiO2/Ti3C2Tx gave a
specific capacitance was doubled, synergistically benefiting from the specific capacitance of 143 F g1 at 5 mV s1, 1.5 times as high as sole
improvements of the conductivity and pseudocapacitance.201 Yang et al. Ti3C2Tx.219 A facile and controllable route to prepare high performance
reported a series of typical work about doped MXenes. Firstly, N-doped Ti3C2/MnO2 electrode materials was developed by Geng et al.174 A
delaminated Ti3C2Tx electrode materials exhibiting a high-capacity molecularly stacked structure of Ti3C2Tx/MnO2 was realized by taking
(266.5 F g1 at 5 mV s1 and 126 F g1 at 2 A g1) in 6 M KOH solu- the advantages of the good compatibility of both colloidal systems, and
tion was reported.202 They further co-doped Ti3C2Tx with N and S (both the novel hybrid electrode showed top-ranking electrochemical perfor-
provided by thiourea), and obtained much enhanced performance mance (8.3 W h kg1 at 221.33 W kg1, and 2376 W kg1 at
(175 F g1 at 2 mV s1 in Li2SO4 solution).203 Also, flexible 3.3 W h kg1) when tested in a flexible and symmetric supercapacitor. In
nitrogen-doped 2D titanium carbides films were prepared by an ex-situ addition, Ti3C2Tx@MFNDs with a 3D interpenetrating assembly by
solvothermal method, and the obtained films exhibited an ultrahigh confining MnFe2O4 nanodots (MFNDs) in hierarchically layered
volumetric capacitance of 2836 F cm3 (927 F g1) at 5 mV s1 in Ti-MXene (Ti3C2Tx) has been developed, which showed a high energy
3 M H2SO4 solution.204 density (62.95 W h kg1), a high power density (7000 W kg1), as well as
The surface terminations of MXenes also show important influence on remarkable rate and cycling performance.220 Conductive polymers were
the electrochemical properties. Dall’Agnese et al.205 replaced the termi- also an effective ingredient for increasing the performance of
nal fluorine with oxygen-containing functional groups after the chemical MXene-based composite electrodes.167,211,221–223 Typically, Wang et al.
intercalation of potassium salts, which led to a 4-fold increase in the explored polyaniline and V2C MXene composite nanomaterials firstly,
capacitance. In addition, delamination of Ti3C2Tx layers led to both an named as PANI/MXene, and constructed high energy density super-
increase of the specific surface area of MXene films and the modification capacitor and high sensitivity ammonia sensor successfully.224 PAN-
of the surface chemistry of d-Ti3C2Tx. Stable capacitance of 415 F cm3 I/MXene offered a capacitance of 337.5 F g1 at 1 A g1, and the
8
Table 2
Performance of MXene-based materials as supercapactor electrodes.
Electrode materials Electrolyte Specific capacitance Rate performance Cycle stability Potential Configuration Year/
window (V) Ref
MXene/BP thin film 1.0 M H2SO4 896.87 F cm3 at 241.2 F cm3, at 91.74% at 10 A cm3 0–0.8 Three-electrode 2021214
0.69 A cm3 6.94 A cm3 for 10000 cycles system
Porous oxidation- 3 M H2SO4 393 F g1 at 2 mV s1 129 F g1 at 10 V s1 95.7% at 200 mV s1 0–1.7 Three-electrode 2021218
resistant MXene/ after 10000 cycles system
graphene
PANI0.7/MXene film 1 M H2SO4 231.4 F cm3 (82.6F g1) 308 F g1 at 5 mV s1 and 87.5% at 20 mA cm2 0.2–0.8 Three-electrode 2021216
at 10 mV s1 228 F g1 at 100 mV s1 after 5000 consecutive system
charge/ discharge
cycles
PANI/MXene 1 M H2SO4 337.5 F g1 at 1 A g1 337.5, 321.7, 311.2, 97.6% at 5 A g1 after 0–1.5 Three electrode 2021224
301.2, 294.3 and 10000 cycles system
292.5 F g1 at 1, 2, 5, 10,
15 and 20 A g1
MSE-etching Ti3C2Tx 1 M H2SO4 225 F g1 at 1.0 A g1 205 F g1 at 10 A g1 100% at 10 A g1 after 0.55–0.2 Three-electrode 2021206
after treated in 10000 cycles system
LiCl–KCl
Mo1.33CTz-Ti3C2Tz 1 M H2SO4 1200 F cm3 (400 F g1) at 875 F cm3 (282 F g1) at 100% at 10 A g1 after 0.5–0.2 Three-electrode 2021225
10 A g1 and 864 F cm3 20 A g1 27000 cycles stainless-steel and
(288 F g1) at 100 A g1 plastic Swagelok cells
Ti3C2–Cu 1.0 M H2SO4 885.0 F g1 at 0.5 A g1 131.6 F g1 at 10 A g1 in 89% at 2 A g1 after 0–1.6 Symmetric two- 2021209
1 M KOH 10000 cycles electrode system
NiCo2- 2 M KOH 332.2 mAh g1 (240 F g1) 165 F g1 even at 87.5% at 5 A g1 after 0–1.4 Three-electrode 2020226
LDHs@MXene/ at 1 A g1 165 F g1 20 A g1 5000 cycles system
rGO
3D porous Ti3C2Tx/ 3 M H2SO4 375 F g1 at 5 mV s1 251.2 F g1 at 95.9% at a 10 A g1 0.7–0.3 Three-electrode 2020189
carbon nanotubes 1000 mV s1 after 10000 cycles system
(CNTs) film
MXene/PANI 1 M H2SO4 556.2 F g1 at 0.5 A g1 437.7 F g1 at 5 A g1 91.6% at 5 A g1 after 0.2–0.6 Three-electrode 2020223
5000 cycles system
Fig. 8. MXene based composites for (a) Li-ion battery, (b) Na-ion battery, (c) K-ion battery. Reproduced with permission from (a) Ref. 244, (b) Ref. 230, (c) Ref. 232.
capacitance of the devices can remain 97.6% after 10000 cycles, developing. Shown in Fig. 8 are the representative MXene-based elec-
implying huge possibilities for practical applications. trode materials for these secondary batteries. MXenes can provide high
More work toward improving the performance of MXene-based electrical conductivity, low operating voltage (0.2 to 0.6 V vs. Li/Liþ)
supercapacitor electrodes has been continuously reported, and as more and low diffusion barriers for Li ions, delivering excellent rate perfor-
improvement achieved, researchers may find a significant place for the mance and cycling stability.23 Theoretically, MXenes should have a
flexible electrodes made from MXene/polymer in the incoming portable higher specific capacity, but the experimental results are often inferior to
electronics. To provide a convenient reference for the researchers in this theoretical values. For example, the specific capacity for V2CTx used as
area, the typical investigations and their features are summarized and LIB electrode was theoretically calculated as high as 940 mA h g1,240 but
listed in Table 2. the measured value was just 252 mA h g1,241 and the initial Coulombic
efficiency (CE) is low. The unsatisfactory performance can be mainly
3.2. Metal-ion batteries ascribed to the following reasons. Firstly, restacking of MXene nano-
sheets happens during synthesis and testing, which results in the decrease
Much work on the MXene-based electrodes for secondary batteries of the MXenes surface area and the increase of resistance between MXene
are focused on lithium-ion batteries (LIBs),36,94,227,228 although appli- layers. Secondly, the terminations attached to the MXene surfaces
cations of MXenes on other kinds of secondary batteries such as sodium, consume part of Li ions, resulting in the low CE.242,243
potassium, zinc, aluminum and magnesium ion batteries (SIBs,229,230 A number of strategies have been developed to enhance the electro-
PIBs,231–233 ZIBs,234–236 AIBs237,238 and MIBs239) are also vigorously chemical performance of MXene electrodes for LIBs, including surface
9
Table 3
Performance of MXene-based materials as secondary battery electrodes.
Electrode materials The The initial charge/ Cyclability (mA h g1) Rate capability (mA h g1) Potential Year/
first discharge capacities window (V) Ref.
C.E. (mA h g1)
Co–NiS/MXene-LIBs 57.4 978/1704 at 1120 at 0.1 A g1 after 200 1072, 853, 637, 353, 156, and 72 at 0.1, 0.2, 0.5, 0.01–3.0 2021251
0.1 A g1 cycles 1, 2, and 5 A g1
MOFs-CoP@MXene- 69.6 644.7/926.3 at 706.5 at 0.2 A g1 after 200 818.6, 655.9, 594.1, 450.0, 328.4 and 219.1 at 0.01–3.0 2021244
LIBs 0.2 A g1 cycles, 585.8 at 0.5 A g1 after 100, 200, 500, 1000, 2000 and 5000 mA g1
1000 cycles
Fe–Ti3C2Tx-LIBs 88.2 610/691.8 at 418.8 at 0.2 A g1 after 500 564.9, 400, 260.2, 183.7 and 109.8 at 50, 100, 0.01–3.0 2021252
0.2 A g1 cycles (10 C) 200, 300 and 500 mA g1 under 10 C
CoCH@MXene-LIBs 64.1 717.7/1118.2 at 733.6 at 1 A g1 after 500 cycles 830.6, 696.3, 493.5, 364.5, and 253.0 at 0.1, 0.2, 0.01–3.0 2021253
0.1 A g1 0.5, 1, and 2 A g1
LTP-TiO2/MXene-LIBs 50 233/466 at 193 at 0.1 A g1 after 500 cycles 204 and 94 at 0.05 and 1 A g1 0.01–3.0 2021254
0.05 A g1
MoS3–Ti3C2Tx-LIBs 68 916/1347 at 568 at 2 A g1 after 1000 cycles 982, 948, 925, 824 and 677 at 0.1, 0.2, 0.5, 1, and 0.01–3.0 2021255
0.2 A g1 2 A g1
SnS/Ti3C2Tx-LIBs 86.04 1079.2/1254.3 at 866 at 0.5 A g1 after 300 cycles 1025.1, 935.4, 902, 860, and 787.7 at 0.1, 0.5, 1, 0.01–3.0 2020256
0.1 A g1 2, and 5 A g1
Si p-NS@TNSs-LIBs 80.2 2077/2588 at 501 at 1 A g1 after 2000 cycles 1498, 1331, 1248, 1161, 1054, and 899 at 0.1, 0.01–2.0 2020257
0.2 A g1 0.2, 0.5, 1, 2, and 4 A g1
SiO2/MXene-LIBs 69.9 820/1173 at 635 at 1 A g1after 200 cycles 840, 739, 683, 553, and 517 at the rates of 0.1, 0.01–3.0 2020258
0.2 A g1 0.5, 1, 2, and 3 A g1
S-TC (SnS2/Sn3S4 52.4 707/1348 at 462.3 at 0.1 A g1 after 100 601.3, 540.4, 479.4, 423.9, 352.2, 216.5 at 0.1, 0.005–3 2020259
hybrid Ti3C2) -LIBs 0.1 A g1 cycles 0.2, 0.5, 1, 2 and 5 A g1
Si/d-Ti3C2-LIBs 74.1 1789.8/2415.4 at 1137.6 at 0.5 A g1 after 200 1948, 1620, 1310, 890 at 0.2, 0.5, 1 and 2 A g1 0.01–1.0 2019260
0.5 A g1 cycles
V4C3Tx-BM–HF–LIBs 62.6 376.2/600.8 at 225 at 0.1 A g1 after 300 cycles 339.8, 268.3, 191.7, 130.9, 100.5, 78.9, and 0.01–3.0 2019261
0.1 A g1 49.2 at 0.1, 0.2, 0.5, 1, 1.5, 2, and 3 A g1
3D porous MXene 65.5 455.5/695.4 at 314.9 at 0.05 A g1 after 300 215.6, 187.4, 133.3, 112.5, and 101 at 1, 2, 10, 0.01–3.0 2019262
foams-LIBs 0.05 A g1 cycles, 220 and 180 at 1 and 15, and 18 A g1
2 A g1 after 3500 cycles
V2C@Sn-LIBs 51.24 1115.6/1284.6 at 1262.9 at 0.1 A g1 after 90 941, 690.8, 482.7, 393.2, 317.5, 279.7 and 0.01–3.5 2019263
0.1 A g1 cycles 205.2 at 0.3, 1, 3, 5, 8, 10 and 20 A g1
MXene-derived TiO2/ 82.8 288/348 at 0.5C 130.6 at 10C after 1000 cycles 302.8, 229.1, 200.4, 185.2, 170.7, 148.4128.3 1.0–3.0 2019264
RGO-LIBs and 111.4 at 0.5, 1.0, 2.0, 5.0, 10, 20 50 and 100C
(1.0C ¼ 168 mA g1)
Ti3C2/Si-LIBs 61.1 2145.1/3512.5 at 973 at 1 A g1 after 800 cycles from 1849 to 467 at from 0.1 to 2 A g1 0.01–3.0 2019265
0.1 A g1
KOH porous MXene 42.4 188 at 0.1 A g1 after 1500 195 and 83.85 at 0.05 and 5 A g1 0.005–3.0 2021266
monolith-SIBs cycles
Co–NiS/MXene-SIBs 66.1 609/922 at 0.1 A g1 510 at 0.1 A g1 after 43 cycles 541, 497, 461, 422, 370, and 263 at the current 0.01–3.0 2021251
density of 0.1, 0.2, 0.5, 1, 2, and 5 A g1
a-VOx/V2C-SIBs 97.7 300/307 at 54 at 2 A g1 after 1800 cycles 310, 271 and 96 at 0.05, 0.1, 2.0 A g1 1.5–3.8 2021230
0.05 A g1
Nb2CTx@MoS2@C-SIBs 56.9 580/1020 at 403 at 1 A g1 after 2000 cycles 572, 561, 544, 506, 480, 454, 340 and 260 at 0.1, 0.01–3.0 2021267
0.1 A g1 0.2, 0.5, 1, 2, and 5, 20 and 40 A g1
f-Ti3C2/NiCo2Se4-SIBs 77.8 409.2/526.2 at 379.2 at 0.1 A g1 after 100 594.3, 399.4, 376.7, 351.1, 333.7, 316.5 and 0.01–3.0 2021268
0.5 A g1 cycles 289.1 at 0.05, 0.1, 0.2, 0.5, 1, 2 and 5 A g1
MXene@NCRib-SIBs 50.1 398.6/795.5 at 210.2 at 1.0 A g1 after 1000 340.1, 275.4, 240.6, 206.6, 169.9, and 113.5 at 0.01–3.0 2021269
0.1 A g1 cycles 0.1, 0.2, 0.5, 1, 2, and 5 A g1
Na2.0Ti3C2Tx-SIBs 89.5 197/220 at 72 at 1.0 A g1 after 100 cycles 177, 161, 146, 132, 107 and 78 at 0.02, 0.05, 0.1, 0.001–3.0 2021270
0.02 A g1 0.2, 0.5 and 1.0 A g1
Cu1.75Se-MXene-CNRib- 58.37 678.6/1162.4 at 480.7 at 1 A g1 after 1000 611.2, 519.5, 451.0, 392.8, and 355.3 at 0.1, 0.2, 0.01–3.0 2021271
SIBs 0.1 A g1 cycles 0.5, 1.0, 2.0 and 5.0 A g1
o-P-CoTe2/MXene-PIBs 72.9 622.7/853.8 at 373.7 at 0.2 A g1 after 200 420.7, 366.8, 313.7, 279.6, 222.5, 195.8, and 0.01–2.6 2021232
0.2 A g1 cycles 168.2 at 0.2, 0.5, 1, 2, 5, 10, and 20 A g1
MXene@NCRib-PIBs 201.5 at 1.0 A g1 after 1000 371.1, 281.4, 220.3, 180.7, 138.1, and 60.7 at 0.01–3.0 2021269
cycles 0.1, 0.2, 0.5, 1.0, 2.0, and 5.0 A g1
Sb/Na–Ti3C2Tx-PIBs 65.6 651.6/993.3 at 392.2 at 0.1 A g1 after 450 558.9, 359.6, 252.8, 182.5, and 127.0 at 0.1, 0.2, 0.01–3.00 2021272
0.1 A g1 cycles 0.5, 1.0 and 2.0 A g1
MXene-derived TiOxNy/ 28.1 185/658 at 0.2 A g1 150 at 0.2 A g1 after 1250 765, 127, 102, 84 and 72 at 0.1, 0.2, 0.4, 0.8 and 0.01–3.0 2021233
C-PIBs cycles 1.6 A g1
MXene-derived TiO2/ 75.6 282/373 at 91.0 at 1.0 A g1 after 1000 354.3, 282.2, 220.9, 151.7 and 107.1 at 0.05, 0.1, 0.1–3.0 2021264
RGO-PIBs 0.05 A g1 cycles 0.2, 0.5 and 1.0 A g1
K–V2C@MnO2-ZIBs 240.7 at 2.0 A g1 after 5000 316.3, 208.3 and at 0.3, 2.0 and 15.0 A g1 0.8–1.8 2021273
cycles
MXene-coated Zn-ZIBs 205.5 at 1.0 A g1 after 500 281.2 and 145.7 at 0.2 and 3.0 A g1 1.0–1.8 2021274
cycles
H2V3O8/MXene-ZIBs 99.7 340/340.9 at 159.3 at 5 A g1 after 5600 365.3, 341.4, 321.2, 297.7, 240.2 and 163.8 at 0.2–1.6 2021234
0.2 A g1 cycles 0.2, 0.5, 1, 2, 5 and 10 A g1
1.8-V2CTx-ZIBs 97.3 412/423.5 at 283.7 at 30 A g1 after 2000 386, 378, 371, 365, and 358 at 10, 15, 20, 25, and 0.25–1.6 2020235
1.0 A g1 cycles 30 A g1
10
Fig. 9. Illustration of the developing course of mechanism for MXenes as the inhibitor to suppress the polysulfide shuttling. (a) Chemical adsorption or bonding of
polysulfides to Ti2CTx through Ti–S bonds and the corresponding XPS results. (b) Two-step interaction between the –OH functionalized MXenes and polysulfides,
including the formation of thiosulfate and Lewis acid–base interactions. (c) Formation process and XPS analysis verification of a sulfate complex protective membrane
on the Ti3C2Tx MXenes surface. Reproduced with permission from (a) Ref. 297, (b) Ref. 298, (c) Refs. 299, 300.
modification, intercalation and compositing. According to the first- 1076.7–370.6 mA h g1 for the varying current densities of 0.1–10 A g1
principles calculations, a large value of specific capacity up to 1264/ and superior long cycle capability of 562 mA h g1 at 5.0 A g1 for 800
1767 mA h g1 can be expected by replacing –O terminations with –P/–Si cycles without degradation. Three dimensional (3D) TiO2@ni-
terminations in MXenes.245 This prediction means that further explora- trogen-doped carbon (NC)/Fe7S8 composite was fabricated by Zhang et
tion of surface modification would be very fruitful to greatly increase the al. They employed a facile and simple hybrid strategy via in situ poly-
capacity of MXene electrodes of LIBs. In Lu's work,246 the calcium ions merization of pyrrole monomer with alkalized Ti3C2Tx and subsequent
were introduced into the interlayer of V2CTx via alkalization and vulcanization at 700 C, and the as-fabricated composite demonstrated a
ion-exchange. Thus, a larger interlayer spacing was obtained, offering an high reversible capacity, excellent rate capability and robust long cycling
efficient Liþ transport channel. Moreover, the process of ion-exchange stability in lithium-ion batteries.248
enhanced electron conductivity by reducing –F surface groups and also SIBs and PIBs are competitive candidates for next generation energy
promoted surface terminations of the V2CTx to participate into redox storage devices due to their rich abundance and low cost in materials.
reaction. As a result, the V2CTx-Ca withstood 200 cycles at 0.5 C, However, they are currently facing significant challenges of lacking op-
retaining a capacity of 500 mA h g1. Zhang et al. designed and fabri- timum electrode materials. Some work indicated that the structure of
cated a new anode material of NiCo-LDH nanosheet anchored on the MXenes has a desirable sodium ion insertion/extraction kinetics, and the
surface of Ti3C2Tx (NiCo-LDH/Ti3C2Tx).247 The layered NiC- volume change upon cycling is quite small.249,250 Compared with
o-LDH/Ti3C2Tx greatly reduced the volume expansion of NiCo-LDH lithium-ion batteries, other metal-ion batteries depends largely on its
during Li ion intercalation. As a result, the as-designed NiC- cathode structure and electrolyte properties. As one kind of layered and
o-LDH/Ti3C2Tx exhibited excellent rate capacities of 2D materials, MXenes have received extensive attention as battery
11
Fig. 10. MXene-based hierarchical structures as sulfur host for high-performance Li–S battery. (a) Versatile 3D printed framework comprising nitrogen-doped porous
Ti3C2Tx competent in regulating dual electrodes. (b) Porous N-doped Ti3C2 MXene serves as an effective immobilizer and a multifunctional electrocatalyst. (c) PA-
MXene/CNT aerogel by the unidirectional freeze-drying. (d) Schematic illustration of discharging/charging process of OV-TnQDs@PCN/S. Reproduced with
permission from (a) Ref. 279, (b) Ref. 301, (c) Ref. 303, (d) Ref. 309.
electrodes. For example, theoretical calculations found the great poten- 3.3. Lithium sulfur batteries
tial (351.8 mA h g1) of Ti3C2Tx electrode for SIBs,249 implying a big
chance for MXenes to be applied in SIBs.164 The tunable interlayer As one type of the promising electrochemical energy storage devices,
spacing of MXenes can effectively mitigate the volume expansion rechargeable lithium–sulfur (Li–S) secondary batteries have different
induced by Kþ insertion and lower the intercalation barrier, but it also energy storage mechanism and electrode materials from the conventional
has the similar problem of low specific capacity with SIBs. Similar stra- ones such as lithium-ion batteries (LIBs), sodium-ion batteries (SIBs), and
tegies developed to prepare enhanced MXene-based LIBs’ electrodes potassium-ion batteries (PIBs). Their high theoretical specific capacity
have been applied to SIBs and PIBs. The typical work on these metal-ion (1675 mA h g1) and energy density (2500 W h kg1) make them an
batteries in recent years is summarized in Table 3, presenting the attractive and promising candidate for next-generation energy storage
composition of the electrodes, their performance and some other high- systems.275 MXenes exhibit promising potential for high-performance
lights to provide an overview of the development in this area. Li–S batteries as sulfur host,44,276,277 interlayer for modifying
Fig. 11. MXene-based interlayer for modifying Li–S battery separator. (a) MXene membrane with abundant in situ formed pores was synthesized through a facile
“oxidation etching” method. (b) Multi-functional separator composed of MXene debris coated eggshell membrane (MXene/ESM). (c) Polysulfides trapping and
conversion process on Ti3C2@iCON-PP and Ti3C2-PP. (d) Schematic illustration of the Ti3C2Tx-PP separators with different mass loading. Reproduced with permission
from (a) Ref. 280, (b) Ref. 278, (c) Ref. 314, (d) Ref. 315.
12
separator,278–280 and lithium anode,281–290 thanks to its metallic con- growth. In addition, the obtained 3DP N-pTi3C2Tx possessing hierarchi-
ductivity, structural variety, strong chemical adsorption ability to poly- cal porosity enabled good cushion of volume change in dual electrodes.
sulfides, effective catalytic effect for fast kinetics, and inducing effect for Similarly, as shown in Fig. 10b, benefiting from the ample nitrogen
uniform growth of Li.291 However, several obstacles still hinder their doping, excellent electrical conductivity and porous structure, porous
practical applications, including the insulative nature of both active N-doped Ti3C2 MXene (P-NTC) not only served as an effective immobi-
sulfur and the final discharge products (leading to low rate capacity), the lizer for LiPS shuttle but also acted as a multifunctional electrocatalyst to
volume changes approaching to 80% at the cathode during cycling promote both the precipitation and decomposition of Li2S. As a result, the
(affecting the stability of the electrode), and the shuttle effect caused by as-fabricated S/P-NTC cathode exhibited high reversible capacity,
the dissolution of intermediate lithium polysulfide series (Li2Sx, outstanding rate capability and good cyclic stability, and even enabled a
4 ¼ x 6) (resulting in the reduce of Coulombic efficiency and capacity high sulfur mass loading of 8.2 mg cm2.301
fading).292 At present, one of the foremost strategies to alleviate these Besides, carbonaceous materials (CNTs,298,302,303 mesoporous car-
problems is exploiting new sulfur host and separator materials to increase bon,304 rGO,305 etc.) were introduced into MXenes to prevent MXene
the conductivity of the cathode and further improve the sulfur utilization nanosheets from restacking and further improve the electronic conduc-
ratio and cyclic stability via suppressing the shuttle effect. MXenes are tivity. As shown in Figs. 10c,303 the lamellae of MXene/CNT/MXene
finding their significance as sulfur hosts and separators. Herein, the ef- sandwich formed multiple physical barriers, coupled with chemical
forts associated with MXenes made on Li–S batteries are summarized and trapping and catalytic activity of MXenes, effectively suppressing lithium
discussed. polysulfide (LiPS) shuttling under high sulfur loading. Therefore, the
obtained 3D host free of micro-/meso-pores demonstrated a substantially
3.3.1. MXene-based sulfur hosts improved confinement ability for the LiPS. The assembled Li–S battery
Although the research of the MXene based materials used in Li–S delivered a high capacity (712 mAh g1 at 0.5C with a sulfur loading of
batteries is still in its early stage, a host of reports have shown signifi- 7 mg cm2) and a superior cycling stability (only 0.025% capacity decay
cance of this endeavor direction.293,294 The inherently metallic nature per cycle over 800 cycles at 0.5C).
and highly active 2D self-functionalized surfaces of MXenes can chemi- Compared with the nonpolar carbonaceous materials, the introduc-
cally bond the intermediate polysulfides by metal–sulfur in- tion of polar materials in sulfur hosts brings about more edges to improve
teractions,295,296 which satisfies the requirements of sulfur hosts for the chemical capture ability of polysulfide. For examples, the metal ox-
high-performance Li–S batteries. The chemical adsorption or bonding of ides306 and sulfides307 with strong polarity are profited for the chemi-
active sulfur and polysulfides to Ti2CTx, an efficient sulfur host, first re- sorption of polysulfides when introduced into MXene matrix.
ported by Liang et al.,297 through Ti–S bonds (sulfur substituting the –OH Furthermore, introduction of the polar materials can also impede the
functional groups, Fig. 9a), provides a new strategy to suppress the restacking of MXene nanosheets, improve the accessibility of ions and
shuttling of polysulfide and improve the stability of battery cycling.297 electrolyte, and increase the active area for adsorb polysulfides. Utilizing
Nazar's group further explored the surface reactivity of the fact that MXenes are prone to oxide, an efficient sulfur host of TiO2
titanium-containing MXenes (Ti3C2Tx and Ti3CNTx) upon contacting QDs@MXene (TiO2 quantum dots decorated d-Ti3C2Tx) was in-situ grown
polysulfide species, showing that prior to forming Ti–S bond via a Lewis by Gao et al.306 In this composite, TiO2 QDs, a strong polysulfide
acid-base interaction, –OH functional groups on MXene surface are adsorbent, were uniformly anchored on MXenes, acting as spacers to
consumed by the polysulfides due to the formation of thiosulfate prevent d-Ti3C2Tx from restacking and thus ensure rapid ion diffusion
(Fig. 9b).298 This dual-mode behavior (Lewis acid-base interaction and and charge transfer. As a result, the TiO2 QDs@MXene realized a synergy
thiosulfate/polythionate conversion) provides a unique double mecha- between rapid charge transfer and enhanced polysulfide adsorption
nism to entrap polysulfides, improving the cycling performance of the capability, exhibiting significant improvement of rate capability and
resulting Li–S batteries.298 Afterwards, a deeper polysulfide adsorption long-term cyclability even with a high sulfur loading. Besides, as one of
and conversion mechanism has been revealed by Yang's and Zhang's the good conductive and strong polar transition metal sulfide, the 1T
groups.237 As displayed in Fig. 9c, the polysulfides complex derived from phase MoS2 was introduced into MXene matrix, resulting in a 3D hybrid
active sulfur are trapped on the MXenes surface, forming the thiosulfate architecture with hierarchical porous structure, high electrical conduc-
through interacting with the cleaved –OH groups during electrochemical tivity and abundant positively charged S-vacancy defects.308 These
conversion process. Sequentially, a complex protective membrane multiple fascinating merits make the sulfur host exhibit a good poly-
including the polysulfides and thiosulfate is formed and efficiently sulfide adsorption capability and effective suppression of polysulfide
chemisorbed onto the polar MXenes' surface because of the continual shuttling, which are beneficial for enhancing the rate performance and
interaction between the surface groups (such as –OH and/or –O) and alleviating rapid capacity fading of Li–S batteries. In addition, as shown
polysulfides.299,300 in Fig. 10d, an effective polysulfide immobilizer and catalytic promoter
To increase the energy density of MXene-based sulfur cathode, it is was developed by constructing oxygen-vacancy-rich TinO2n1 quantum
necessary to construct electrodes capable of loading more sulfur by dots (OV–TnQDs) decorated on porous carbon nanosheets (PCN) by using
enhancing the porous structure and specific surface area of the sulfur Ti3C2Tx MXene as starting materials.309 The synergistic integration of
hosts. Generally, heterogeneous element doping and combining with composition and morphology endowed the OV–TnQDs@PCN with strong
heterogeneous materials are the advisable strategy to optimize the per- chemisorption and catalytic conversion for LiPSs, with adequate space
formance of MXenes for polysulfide capture as sulfur host. Wei et al. for S loading and volume expansion, and with excellent conductive
proposed a versatile 3D printed (3DP) framework comprising nitrogen- pathways for electron and charge transfer.
doped porous Ti3C2Tx (N-pTi3C2Tx) that was competent in regulating
dual electrodes of Li–S batteries, as shown in Fig. 10a.279 Serving as the 3.3.2. MXene-based interlayer for modifying separator
sulfur host, the 3DP N-pTi3C2Tx offered rapid charge transport and effi- Modifying separator by interlayer design to mitigate the shuttling of
cient Li2Sn immobilization/conversion, thereby inhibiting the polysulfide poysulfides by virtue of physical obstruction and chemical adsorption is
shuttle, boosting the sulfur electrochemistry and consequently, enabling one of the most efficient strategies to enhance the electrochemical sta-
high utilization of sulfur in particular under elevated loadings. Mean- bility of Li–S batteries.280,310–316 As Fig. 11 shows, MXenes have proved
while, the 3DP N-pTi3C2Tx interlayer for Li anode with sizable micro- the superiority as the separator interlayer for confining the sulfur and
channels between the printed filaments and ample meso/macro pores, polysulfide.278,317–320 As a pioneering work, to immobilize polysulfide in
provided sufficient space for massive Li deposition and dissipate the cathode side, Song et al. reported an MXene-functionalized poly-
current density. The adequate exposure of lithiophilic N sites would propylene (PP) separator, which significantly enhanced the rate perfor-
effectively guide the uniform Li nucleation to suppress the dendritic mance and cycling stability because of the physical confinement and
13
Table 4
Summary of MXene-based sulfur host or interlayer modified separator for Li–S batteries.
Sulfur cathode Sulfur Sulfur Separator Initial discharge Rate capacity (mA h g1) Cycling Capacity decay Year/
content loading (mg capacity (mA h capacity (mA ratio (% per Ref
(wt%) cm2) g1) h g1) cycle)
MOFs-CoP@Mxene/S 62.7 1.6–2.0 PP 1138.8/0.2C 493/6C, 854.4/0.5C 796.9/0.2C/ 0.1 2021244

300
MoS3/Ti3C2Tx/S 62.16 ~1.6 PP 1083/0.2C 1008/0.1C, 970/0.2C, 825/ 836/0.2C/ 0.2 2021255
0.5C, 628/1C and 457/2C 100, 463/
2C/400
CNT/S 70 ~1 CoTe-MXene/PP 1664/0.1C 1664/0.1C, 1242/0.2, 696/2C/300 0.09 2021324
1115/0.5C, 1025/1C, 952/
2C, and 905/3C
S@PDA@C–Ti3C2Tx/L- 69.6 4 PP 1560/0.12C 1560/0.12C, 1272/0.3C, 496/3C/ 0.04 2021325
Ti3C2Tx 1127/0.6C, 1042/0.9C, 1000
992/1.2C, 944/1.2C, 895/
2.4C and 854/3C
OV–TnQDs@PCN/S 79.1 2.2 PP 1375/0.05C 1023/0.1C, 889/0.2C, 796/ 660/2C/ 0.012 2021309
0.5C, 718/1.0C, and 672/ 1000
2.0C
PA-MXene/CNT 7 PP 712/0.5C 1118/0.2C, 883/0.5C, 764/ 570/0.5C/ 0.025 2021303
1.0C, 703/1.5C, and 668/ 800
2.0C
Ti3C2Tx-CNTs/S 73 7.2 PP 1368/0.2C 1368/0.2C, 1022/0.5C, 621/1C/500 0.062 2021302
878/1C, 659/2C, 512/3C,
and 345/5C
S/Ketjen Black 2.42 Porous MXene 1329.2/0.1C 1282/0.1C, 1004/0.2C, 535/1C/500 0.07 2021280
(0.4 M)-CNT/PP 861/0.5C, 740/1C, and 677/
2C
CNT/S 76 7.6 Ti3C2@iCON-PP 1417/0.05C 1280/0.1C, 1186/0.2C, 706/2C/ 0.006 2021314
1048/0.5C, 956/1C, 846/ 2000
2C, 771/3C, and 687/5C
CNT/S 1.2 Ti3C2Tx/CNTs-PP 760/1C 621.6/1.2C, 497.4/2.4C, 630/1C/200 0.086 2020315
and 478.1/3.6C
S/Oxi-d-MXene900 49 1.15 Oxi-D-MXene 600- 1408.91/1C 1644.38/0.2C, 470.91/5C 800.71/1C/ 0.14 2020316
coated glass fiber 300
porous N-doped Ti3C2 64 1.4–1.6 PP 1072/0.5C 1325/0.2C, 1082/0.5C, 495.28/2C/ 0.033 2020301
MXene (P-NTC)/S 982/1.0C, 877/2.0C and 1200
792/3.0C
chemisorption of the MXene interlayer barrier.318 Dong et al. developed combination of properties and the ever-increasing chemical and struc-
an all-MXene-based flexible and integrated sulfur cathode (without tural diversity. It is impressive that the research and development on the
additional current collector) by filtrating alkalized d-Ti3C2 on PP sepa- synthesis and applications of MXenes can achieve so much in such short
rator, realizing high-energy and long-cycle Li–S batteries.319 In addition years. They are finding their significant place in electrochemical energy
to modifying PP separators, MXene-decorated glass fibers316,317 and storage application among many other technological areas.
eggshell membranes278 were also used as Li–S battery separators, Currently, the related researches are springing up across a wide sci-
exhibiting a good polysulfide adsorption capability, remarkable rate ca- entific community. As new MAX phases and other precursors are
pacity and cycling stability. Except for bare MXene, some MXene-based continuously discovered and the new preparation methods for MXenes
composites were employed to decorate PP separator, such as the are developed, the diversity of MXenes would be richer. According to the
self-assembled MXene/CNT,315,321 the MOF-derived carbon decorated experience of the authors, the primary directions of research and
N-doped MXene films,322 and MXene nanosheets decorated by in-situ development on the MXenes are as follows. (1) A comprehensive un-
grown TiO2 nanoparticles,323 resulting in functionalized PP separators derstanding on the electrochemical energy storage mechanism of
with good performance in terms of hindering polysulfide shuttle and MXenes, including the influence of surface terminations, would be
accelerating charge transfer for enhanced cyclic stability of Li–S battery. beneficial to designing more practical electrodes. (2) Based on the energy
In summary, the polar–polar interaction between MXenes (compos- storage mechanism and rational design, MXene-based materials with
ites) and polysulfides plays an important role in improving rate perfor- high specific capacity would be expected. (3) More opportunities on
mance and cyclic stability of Li–S batteries. As the mechanism for MXenes MXenes different in composition and structure from Ti3C2Tx have yet to
(composites) as the inhibitor in sulfur hosts and separator interlayers to be explored. (4) To promote its commercialization, safer and eco-friendly
alleviate the polysulfide shuttling is being gradually revealed, the routes using lower cost precursors with higher efficiency need to be
intrinsic electrical conductivity, hydrophilicity, and polarity of MXenes developed, and more investigations on the oxidation behavior of MXenes
(composites) will be fully correlated with the enhanced electrochemical are needed to address their susceptibility to oxidation especially during
performance in Li–S batteries. The application of MXenes in Li–S batte- the preparation phase. (5) Flexible and transparent electrodes are critical
ries has been booming after just several years, and more achievements for the next generation of consumer electronics, and MXenes seem to
would be seen as high quality MXenes are fast developing. The param- have huge potential for this opportunity.
eters and highlights of the typical work about MXenes applied in Li–S
batteries are summarized and contained in Table 4 for a convenient Acknowledgements
reference.
This work was supported by the Grants of National Natural Science
4. Conclusions and perspective Foundation of China (52171033 and 51731004) Natural Science Foun-
dation of Jiangsu Province (BK20201283), and Zhishan Youth Scholar
MXenes stand out among the 2D materials world due to their unusual Program of SEU.
14
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20
Xueqin Xu graduated from Nanjing Tech University. She is ZhengMing Sun received his PhD degree from Institute of metal
currently a second-year master student at school of materials research (IMR), Chinese Academy of Sciences. He is currently a
science and engineering at Southeast University. She is working distinguished Professor in the School of Materials Science and
on developing high-performance electrode materials via eco- Engineering, Southeast University. His research interests cover
friendly methods. the research and development of metallic materials, advanced
ceramics and composites, including their synthesis, character-
ization and applications. Recently, he is leading his group to
investigate and develop advanced materials, including MXene
and other low-dimensional materials, for the application in
energy storage and conversion.
Peigen Zhang obtained his PhD degree from college of engi-

neering at Louisiana State University (Baton Rouge). He works
at the school of materials science and engineering at Southeast
University. His research interests include advance ceramics
(including MAX phase), growth mechanism and mitigation
strategy of metallic whiskers in electronic components, and the
synthesis and applications of low-dimensional materials derived
from layered crystals.
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Materials Reports: Energy 2 (2022) 100080

Contents lists available at ScienceDirect

Materials Reports: Energy

MXenes with applications in supercapacitors and secondary batteries: A

Production and Hosting by Elsevier on behalf of KeAi

MOFs-CoP@Mxene/S 62.7 1.6–2.0 PP 1138.8/0.2C 493/6C, 854.4/0.5C 796.9/0.2C/ 0.1 2021244

References 10.1038/natrevmats.2016.98, 01/17/online https://www.nature.com/articles/n

Peigen Zhang obtained his PhD degree from college of engi-

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