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Otgonbayar, Z.; Yang, S.; Kim, I.; Oh, W. MXenes as Electrode Materials for Supercapacitors. Encyclopedia. Available online: https://encyclopedia.pub/entry/41983 (accessed on 30 August 2024).
Otgonbayar Z, Yang S, Kim I, Oh W. MXenes as Electrode Materials for Supercapacitors. Encyclopedia. Available at: https://encyclopedia.pub/entry/41983. Accessed August 30, 2024.
Otgonbayar, Zambaga, Sunhye Yang, Ick-Jun Kim, Won-Chun Oh. "MXenes as Electrode Materials for Supercapacitors" Encyclopedia, https://encyclopedia.pub/entry/41983 (accessed August 30, 2024).
Otgonbayar, Z., Yang, S., Kim, I., & Oh, W. (2023, March 08). MXenes as Electrode Materials for Supercapacitors. In Encyclopedia. https://encyclopedia.pub/entry/41983
Otgonbayar, Zambaga, et al. "MXenes as Electrode Materials for Supercapacitors." Encyclopedia. Web. 08 March, 2023.
MXenes as Electrode Materials for Supercapacitors
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This entry is adapted from the peer-reviewed paper 10.3390/nano13050919

MXenes have been considered to be potential building blocks for composites for use in energy storage applications due to their distinctive 2D wafer structure and superior electrical conductivity. MXenes have been combined with multiple active ingredients, including metal oxides and conductive polymers, to produce a synergistic effect. The synthesis method of MXene shows various surface termini and topographies with different energy storage properties, and there have been multiple studies examining surface modification, stoichiometric ratio, and electrode composition control.

synthesis method 2D MXene electrolyte MXene-based electrode

1. Control of Size of MXene Flake

The morphology and structure of MXenes are strongly influenced by the corrosivity of the synthesis conditions. For example, prolonging the etching time produces a more open structure than the HF etching of Ti3AlC2, which produces an accordion-like Ti3C2Tx (MXene). Ti3C2 with a corrosion time of 216 h has a deformed octahedral structure that loses more Ti and C contact on the surface than Ti3C2 with a short corrosion time of 24 h, thus giving it significantly better capacitive achievement [1][2], as shown in Figure 1. However, despite the higher ionic conductivity and easier access to ion diffusion pathways, the smaller MXene fragments have higher electrical conductivity due to the higher resistance to intersurface contact. Kayali et al. [3] examined how the side diameters of MXenes affect their electrochemical properties. In addition, Mustafa et al. [4] demonstrated that rational design electrodes are fabricated by mixing MXene with an aqueous solution of chloroauric acid (HAuCl4). As shown in Figure 1g,h, the etching time had an influential effect on electrochemical properties of MXene. The symmetric supercapacitors made of MXene and AuNPs have shown exceptional specific capacitance of 696.67 F g−1 at 5 mV s−1 in 3 M H2SO4 electrolyte, and they can sustain 90% of their original capacitance for 5000 cycles (in Figure 2). The highest energy and power density of this device, which operates within a 1.2 V potential window, are 138.4 Wh kg−1 and 2076 W kg−1, respectively. From topography analysis, it is clearly shown that Au NPS are homogeneously located on a MXene nanosheet; therefore, the Au NPs served as the best intercalators in the hybrid structure [5]. The thickness of the MXene/AuNPs composite film had stacked layer with a 12 μm thickness.
Figure 1. Schematic illustration of the typical structures of Ti3C2 with the evolution of the etching time: SEM images of the typical as-fabricated MXene with the CV curves and specific capacitance vs. scan rate for the electrodes with different etching times [1][2].
Figure 2. (a) CV curves of MXene at different scan rates in 3-electrode setup; (b) CV curves of MX/AuNPs in 1 M H2SO4 at different scan rates in 3-electrode setup; (c) Nyquist plots of MX/AuNPs with inset showing the equivalent circuit model for the Nyquist plots; (d) MX/AuNPs electrode showing excellent cyclic stability with 98% capacitance retention at 100 mV s−1 1M H2SO4 after 5000 cycles; (e) cross-sectional image of the MX/AuNPs composite film demonstrating stacked layered structure; (f) cross-sectional image showing the thickness of the composite film [5].

2. Category of Composition

Table 1 summarizes most of the previous studies examining Ti3C2Tx and other MXenes for energy storage applications or supercapacitor electrodes. Ti2CTx MXenes [6][7] deliver outstanding outcomes. Compared to carbides, nitride-based MXene exhibits higher electrical conductivity [8]. Accordion-structured, -O/-OH-terminated Ti2NTx nanolayers are obtained by synthesizing the Ti2AlN (MAX) phase by oxygen-assisted molten salt followed by HCl treatment.
Table 1. Capacitive capabilities of different MXene electrode materials for SCs.
Versatility Synthesis Electrode
Assembly		 Electrolyte Capacitance Cycle
Stability		 Ref.
Ti3C2Tx HF etching Ti3AlC2 and DMSO delamination Filtrating into film 1 M KOH 350 F cm−3 no degradation
(10,000 cycles)		 [9]
Ti3C2Tx HCl/HF etching Ti3AlC2 Rolling 1 M H2SO4 900 F cm−3 or 245 F g−1 no degradation
(10,000 cycles)		 [10]
Ti3C2Tx Lewis acidic molten salt etching Ti3SiC2 Rolling 1 M LiPF6-
EC/DMC		 738 C g−1 or 205 mAh g−1 90%
(2400 cycles)		 [11]
Ti3CTx HF etching Ti2AlC Rolling 1 M KOH 517 F cm−3 no degradation
(3000 cycles)		 [6]
Ti3NTx oxygen-assisted molten salt etching Ti2AlN2 and HCl treatment Coating 1 M MgSO4 201 F g−1 140%
(1000 cycles)		 [12]
V2C HF etching V2AlC and TMAOH delamination Rolling 1 M H2SO4 487 F g−1 83% (10,000 cycles) [13]
V4C3Tx HF etching V4AlC3 Coating 1 M H2SO4 ~209 F g−1 97.23% (10,000 cycles) [14]
Nb4C3Tx HF etching Nb4AlC3 and TMAOH
delamination		 Rolling 1 M H2SO4 1075 F cm−3 76% (5000 cycles) [15]
Ta4C3 HF etching Ta4AlC3 Coating 0.1 M H2SO4 481 F g−1 89% (2000 cycles) [16]
Mo2CTx HF etching Mo2Ga2C and TBAOH delamination Filtrating into film 1 M H2SO4 700 F cm−3 no degradation
(10,000 cycles)		 [17]
Mo2TiC2Tx HF etching and DMSO delamination Mo2TiAlC2 Rolling 1 M H2SO4 413 F cm−3 no degradation (10,000 cycles) [18]
Nanolayered Ti2NTx MXene with -O/-OH surface terminations exhibited a capacitance of 200 F g−1 at a scan rate of 2 mV s−1 in 1 M MgSO4 electrolyte, and this MXene material was prepared by HCl treatment on Ti2AlN-MAX phase. In addition to traditional Ti-based MXene materials, members of the MXene family are expanded indefinitely by using M-centered metal alloys to include C- and N-bonded transition metal species, such as Ta- [19] and Mo- [20] based MXenes, which are valued as reliable electrodes for supercapacitor applications. Conductivity, stability, and electrochemical outcomes are all significantly affected by the intrinsic properties of the M and X elements, and the surface finishes significantly affect these qualities as well. On the other hand, since their properties can be modified by options of different M and X components and surface terminals can be managed, there is tremendous potential to develop new MXene with favorable capacity properties. Therefore, considering their potential utility in supercapacitors, newer MXenes with higher electrochemical efficiency are needed. An appropriate synthesis approach, including etching and separation processes, should be optimized for each MAX precursor because it has a unique atomic bond. This is necessary to achieve the desired structure and achievement. There is a need for a large amount of research to investigate new MXene and preparation techniques, which represents an important and difficult task.

3. Heteroatoms Doping and the Control of Surface-Terminus Group

The surface properties and electron acceptability of the material can be changed by heteroatom doping. N-atom has been concluded to be an active heteroatom that affects the electrochemistry of MXenes, and many studies have examined these relationships. The reaction mechanisms can be summarized as follows: by replacing the C-atoms in the C-layer with N-atoms, it has been demonstrated that the distance between layers increases, effectively improving the electrical conductivity [21]. The most commonly used N-doping methods can be classified into heat treatment in ammonia [16], doping in liquid intermediates, water heat treatment [19][22], solvent heat treatment [23], and liquid peeling [24]. For example, as illustrated in Figure 3, a Ti3C2 film with a flexible N-doping layer was prepared by static adsorption and in situ solvent heat treatment using an alcohol solution saturated with urea as a source of N-atoms [23]. In addition, the intercalation of N in MXene increased the distanced of layers, therefore it offers the opportunity to tune the electrochemical properties.
Figure 3. (i) An exemplification of charge storage and film-electrode fabrication of UN-Ti3C2 [23]. (ii) Schematic illustration of film preparation and electrode fabrication of the UN-Ti3C2.
Moreover, Ti2CTx-MXene underwent simultaneous liquid-gas phase delamination and chemical doping with nitrogen [24]. Under inert environs, the NH2CN utilized as a N-source and intercalant was bonded to the Ti2CTx nanosheets, and during heat treatment, a condensation reaction resulted in polymeric carbon nitride (p-C3N4). Solid-state doping was also shown to be possible. N and S co-doped Ti3C2Tx-MXene with a 75 F g−1 at 2 mV s−1 in Li2SO4 electrolyte were produced by pyrolysis of thiourea [25][26]. Nitrogen has been the primary focus of the majority of experiments investigating MXene doping. The potential to alter MXenes has also been demonstrated by using other types of doping atoms, such as metals and heteroatoms. The calculation results show that B-doping improves the stretchability of MXenes, thus making them ideal for use in pliable-electronics [27]. The interlayer spacing, conductivity, and capacitance of MXenes can also be increased by adding metal atoms such as V [28] and Nb [29] doping. As discussed above, chemical modification can be used to fine-tune the properties of MXenes and improve their outcome rate. As vacancies can lead to flaws in the MXene matrix and subsequently affect the structure, surface properties, and activity of MXenes, it may also be a useful strategy for modifying their properties. Novel types of terminus and doped atoms have been added to MXenes as a result of the growing depth of research examining chemical modification techniques [30][31][32][33][34].

4. Fabricating Vertical Alignments

The RGO/Ti3C2Tx MXene-modified fabrics were fabricated by a facile dip-coating and spray-coating method and the schematic illustration of the procedure is shown in Figure 4. The electrochemical performance of RGO and MXene-modified fabrics were characterized via CV tests in two-electrode configuration by using the 1 M H2SO4/PVA gel electrolyte. Figure 4a shows the CV curves of all-solid-state MCF and RMC supercapacitors at a scan rate of 10 mV s−1. The MCF-based supercapacitor shows the smallest enclosed CV curve (almost a line), indicating its inferior charge storage capability. Meanwhile, the charge storage capability was significantly increased after the incorporation of RGO, as the RMC-1 shows an enlarged CV area. In addition, the incorporation of RGO significantly enhanced the CA to 62.9 mF cm−2 for RMC-1, and the CA was further increased to 92.5 mF cm−2, 115.0 mF cm−2, and 258.0 mF cm−2 for RMC-2, RMC-3, and RMC-4, respectively. The increased CA was ascribed to the synergistic effects between the increased electrical conductivity and dominated pseudocapacitance of MXene. The topography images of the RGO/Ti3C2Tx MXene were analyzed by SEM and the obtained images are shown in Figure 4g,h. As shown in the SEM image, the RGO and MXene sheets are compactly filled in the fiber gaps and fiber surfaces, and graphene sheets can be obviously observed in the gaps between the weft yarns and warp yarns.
Efficient longitudinal ion transfer can be achieved by fabricating MXene membrane electrodes from “T-shaped” fragments [35]. The Ti3C2Tx film electrode in the H2SO4 electrolyte showed a capacity ranging from 2 A g−1 to 361 F g−1, and showed a capacity increase of 76% when the current density was increased to 20 A g−1. Table 2 summarizes the design and results of electrodes that can meet the capacity and current efficiency requirements of a supercapacitor. As illustrated in Table 2, the theoretical limit of MXene capacity can be approached by designing a hydrogel framework, while high-speed results can be obtained at a scan rate of up to 10 V s−1 using the porous MXene structure, and high capacity power with a film thickness of up to 200 μm can be obtained using vertically oriented MXene particles. This can confirm the output result. These designs and their combinations have provided new and exciting possibilities for MXene in supercapacitor applications.
Figure 4. Schematic illustration of multifunctional RGO/Ti3C2Tx MXene fabrics, and electrochemical performance of the MCF and RMC fabrics. (a) CV curves of the MCF and RMC at 10 mV s−1. Areal specific capacitance (b) and gravimetric specific capacitance (c) of MCF and RMC. (d) Areal and gravimetric specific capacitance of RMC compared with the reported MXene-modified fibers, yarns, and fabrics. (e) Nyquist plots of MCF and RMC. (f) Four RMC-4 supercapacitors connected in series as a wristband to power a watch. (g,h) SEM images of fabrics [36].
Table 2. Capacitive outcome of MXene electrodes with optimized structural design.
Electrode Preparation Electrolyte Capacitance Cyclability Ref.
Controlling flake size
Ti3C2Tx film Mixing large and small flakes 3 M H2SO4 435~86 F g−1 10,000 cycles [37]
Adding spacer between MXene interlayer
75 μm Ti3C2Txpillared by
hydrazine		 Suspending in
hydrazine		 1 M H2SO4 250~210 F g−1 no decay
(10,000 cycles)		 [38]
Ti3C2Tx/graphene 3% film Mixing and filtration 3 M H2SO4 438~302 F g−1 no decay [39]
Sandwiched Ti3C2Tx/CNT 5%
film		 Alternative filtration 1 M MgSO4 390~280 F cm−3 no decay [40]
V2CTx/alkali metal cations film Cation-driven
assembly		 3 M H2SO4 1315~>300 F cm−3 106 cycles [41]
Ti3C2Txionogel film Immersing into EMITFSI EMITFSI 70~52.5 F g−1 1000 cycles [42]
Ti3C2/CNTs film Electrophoretic
deposition		 6 M KOH 134~55 F g−1 no decay [43]
carbon-intercalated Ti3C2Tx In situ carbonization 1 M H2SO4 364.3~193.3 F g−1 10,000 cycles [44]
Ti3C2Tx@rGO film Plasma exfoliation PVA/H2SO4 54~35 mF cm−2 1000 cycles [45]
Designing 3D/porous structure
13 μm Ti3C2Tx film 1~2 μm PMMA template 3 M H2SO4 310~100 F g−1 - [46]
MXene/CNTs film Ice template 3 M H2SO4 375~92 F g−1 10,000 cycles [47]
Ti3C2 aerogel assembly and
freeze-drying		 1 M KOH 87.1~66.7 F g−1 10,000 cycles [48]
Ti3C2Txhydrogel assembly
and freeze-drying		 H2SO4 370~165 F g−1 10,000 cycles [49]
Ti3C2Tx/carbon cloth Freeze-drying with KOH treatment 1 M H2SO4 312~200 mF cm−2 8000 cycles [50]
Ti3C2Tx/Ni foam Electrophoretic deposition 1 M KOH 140~110 F g−1 10,000 cycles [51]
Compact and
nanoporous
Ti3C2Tx film		 Freeze-drying and
mechanically pressing		 3 M H2SO4 932~462 F cm−3 5000 cycles [52]
3D porous Ti3C2Tx film Reduced-repulsion freeze casting
assembly		 3 M H2SO4 358.8~207.9 F g−1 10,000 cycles [53]
Fabricating vertical alignments
Anti-T Ti3C2Tx film Filtrating through an entwined
metal mesh		 1 M H2SO4 361~275 F g−1 10,000 cycles [33]
200 μm Ti3C2Tx film Mechanical shearing of a discotic lamellar
liquid-crystal
MXene		 3 M H2SO4 >200 F g−1 20,000 cycles [32]

5. 3D Microporous Sphere/Tube Ti3C2Tx

Due to strong van der Waals interactions, both V- and Ti-based MXenes tend to re-stack, resulting in decreased surface area and potassium ion kinetics, and many methods have been developed to fabricate 3D architectures using PICs in attempts to solve this problem. To generate 3D microporous spheres or tubes made of Ti3C2Tx, Fang et al. devised a facile spray-lyophilization process [54]. Figure 5a,b shows a 3D Ti3C2 structure consisting of several smooth-surfaced spheres and some tubes. The development of 3D morphology successfully solved the stacking problem of MXene nanosheets and enabled the possibility of fast ion transport (Figure 5c). The constructed PICs offered significant energy density and power density (98.4 Wh kg−1 and 7015.7 W kg−1). According to Figure 5d,e, Zhao et al. 3D K-pre-intercalated Ti3C2Tx (MXene) (K-Ti3C2Tx) was synthesized by electrostatic flocculation, freeze-drying, and KOH treatment, and the MXene interlayer gap escalated to 1.32 nm after K-intercalation, which was advantageous for the K+ kinetics. The proposed PICs exhibited an energy density of 163 Wh kg−1 and a high power density of 8.7 kW kg−1 with the combination of an AC cathode with a 3D K-Ti3C2Tx anode. In addition to the above study, the Zhang et al. research group fabricated a 3D foam-like 3D FMS by electrostatically neutralizing Ti3C2Tx with positively charged melamine followed by calcination [43], where the K conductivity was accelerated due to a surface area of 89.5 m2 g−1. Figure 5f shows the schematic illustration of the synthesis procedure of the 3D-FMS nanocomposites.
Figure 5. (a,b) SEM images. (c) An exemplification of ion transport in 3D and 2D Ti3C2 electrodes [55]. (d) An exemplification of fabrication [56] and (e,f) the synthesis of 3D-FMS [57].

6. Design of 3D Porous MXene Electrode

By assembling 2D MXene wafers into a 3D electrode structure, the achievement of MXene materials for energy storage applications can be improved. The design of the MXene 3D foam was completed using a variety of technologies. Therefore, it is advantageous to reduce the size of the fragment and increase the interlayer distance so that the transport and accessibility of ions to the active site can be improved to increase the efficiency of MXene. However, by forming a 3D/porous electrode structure with large active surfaces that are accessible to ions as well as interconnected holes for ion-transport channels, the high throughput potential of MXene can be increased further. The achievement of MXene is expected to increase as appropriate porous structures can provide paths for electrolyte wetting and ion transport, thus reducing electrical resistance and shortening diffusion distance. Porous MXene electrodes have been generated by a variety of methods, such as chemical etching [58], template method [59], hydrazine-induced foaming [60], and electrical deposition [61]. Recently, small ice particles have been used as a self-sacrificing template for forming a flexible MXene/CNT film having large pores and nanopores. The controlled porous structure allows for capacities up to 375 and 251 F g−1 at 5 and 1000 mV s−1, respectively. Foaming, corrugation, and carbon assembly have also been suggested to be effective ways to create porous MXene frameworks [62][63][64][65].
It is also possible to combine 3D MXene aerogels with graphene [43]. As shown in Figure 6, both GO/MXene nanosheets are forced to gradually arrange along the ice crystal boundary during the lyophilization of the mixed GO and MXene solution, and they are eventually crosslinked through interactions to create a 3D lattice porous structure.
Figure 6. An exemplification of fabrication of (a) aerogel, (b) MSCs, (c) photo of NCs in dispersion of water, (d) size of MXene flake, and (e) pressure-strain curve [66].

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Subjects: Electrochemistry
Contributors MDPI registered users' name will be linked to their SciProfiles pages. To register with us, please refer to https://encyclopedia.pub/register :
Zambaga Otgonbayar
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Sunhye Yang
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Ick-Jun Kim
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Won-Chun Oh
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Update Date: 09 Mar 2023
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