Advances in MXene Films: Synthesis, Assembly, and Applications

Li, **aohua; Ran, Feitian; Yang, Fan; Long, Jun; Shao, Lu

doi:10.1007/s12209-021-00282-y

Advances in MXene Films: Synthesis, Assembly, and Applications

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Published: 07 March 2021

Volume 27, pages 217–247, (2021)
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Advances in MXene Films: Synthesis, Assembly, and Applications

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**aohua Li¹,
Feitian Ran¹,
Fan Yang¹,
Jun Long¹ &
…
Lu Shao¹

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Abstract

A growing family of two-dimensional (2D) transition metal carbides or nitrides, known as MXenes, have received increasing attention because of their unique properties, such as metallic conductivity and good hydrophilicity. The studies on MXenes have been widely pursued, given the composition diversity of the parent MAX phases. This review focuses on MXene films, an important form of MXene-based materials for practical applications. We summarized the synthesis methods of MXenes, focusing on emerging synthesis strategies and reaction mechanisms. The advanced assembly technologies of MXene films, including vacuum-assisted filtration, spin-coating methods, and several other approaches, were then highlighted. Finally, recent progress in the applications of MXene films in electrochemical energy storage, membrane separation, electromagnetic shielding fields, and burgeoning areas, as well as the correlation between compositions, architecture, and performance, was discussed.

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Introduction

Since the discovery of mechanically exfoliated graphene in 2004 [1], research on ultrathin two-dimensional (2D) nanomaterials has grown exponentially in the fields of materials, material chemistry, and nanotechnology. Following graphene, a variety of 2D nanomaterials, such as antimonene [2, 3], phosphorene [4], hexagonal boron nitride [5], transition metal disulfides [6], layered metal oxides, and layered double hydroxides, have been reported [38]. Additionally, the properties of MXenes can be tuned by the types and ratios of M to X elements. Furthermore, the advanced characterizations of the MXene-based materials further reveal their potential properties, which facilitate and guide their studies and processing.

Unlike graphite layers maintained by weaker Van der Waals forces, the adjacent layers of MAX are held together by strong covalent bonds or metal bonds. As a result, it is difficult to etch directly by a conventional etchant to produce T₃C₂ sheets. Two-dimensional MXene sheets were not successfully achieved until the Ti₃AlC₂ powders were added to a concentrated HF solution by Gogotsi's group [23]. By combining geometry optimization and XRD analysis of the treated Ti₃AlC₂ powders, Gogotsi et al. [23] concluded that the Al layers could be dissolved by the HF acid solution and replaced by functional groups (mainly –F and –OH), leaving a structure with a chemical formula of Ti₃C₂. The etching procedure is illustrated in Fig. 2, and the mechanism can be described by the following formulas:

$${{\text{Ti}_3\text{AlC}_2 + 3\text{HF}}} \to {\text{AlF}}_{{3}} { + 1}{\text{.5H}}_{{2}} {{ + \text{Ti}}}_{{3}} {\text{C}}_{{2}}$$

(1)

$${{\text{Ti}_3\text{C}_2 + 2\text{H}}}_{{2}} {\text{O}} \to {{\text{Ti}_3\text{C}_2}}\left( {{\text{OH}}} \right)_{{2}} {\text{ + H}}_{{2}}$$

(2)

$${{\text{Ti}_3C_2 + 2\text{HF}}} \to {{\text{Ti}_3\text{C}_2\text{F}}}_{{2}} {{ + \text{H}}}_{{2}}$$

(3)

Similarly, Lin et al. [39] successfully fabricated 2D ultrathin Ta₄C₃ MXene sheets with nanosized lateral dimensions using a two-step liquid exfoliation strategy. The etching process can be described as:

$${\text{Ti}}_{{4}} {\text{AlC}}_{{3}} {\text{ + 3HF = AlF}}_{{3}} {\text{ + Ta}}_{{4}} {\text{C}}_{{3}} { + 1}{\text{.5H}}_{{2}}$$

(4)

$${\text{Ta}}_{{4}} {\text{C}}_{{3}} {\text{ + 2H}}_{{2}} {\text{O = Ta}}_{{4}} {\text{C}}_{{3}} {\text{(OH)}}_{{2}} {\text{ + H}}_{{2}}$$

(5)

$${\text{Ta}}_{{4}} {\text{C}}_{{3}} {\text{ + 2HF = Ti}}_{{4}} {\text{C}}_{{3}} {\text{F}}_{{2}} {\text{ + H}}_{{2}}$$

(6)

$${\text{Ta}}_{{4}} {\text{C}}_{{3}} {\text{ + O}}_{{2}} {\text{ = Ta}}_{{4}} {\text{C}}_{{3}} {\text{O}}_{{2}}$$

(7)

Although the HF etching method is widely used in the production of Ti₃C₂T_x, its practical application is still severely hindered because of the toxicity and harmfulness of HF [40,41,42,43]. Compared with the direct usage of a concentrated HF solution, the in situ produced HF can remove the A atom layers via a similar reaction process, which suggests protons and fluoride ions are necessary for etching Ti₃AlC₂ powders. The in situ HF etching of MAX can produce large fractions of single-layered MXene flakes with high yields. The obtained MXene sheets are usually accompanied by larger sizes and fewer nanometer-size defects, which are important for some applications. For example, large flakes with few defects are more suitable for applications requiring high electrical conductivity [44]. Furthermore, cations (i.e., Li⁺, NH₄⁺) in the etching system can intercalate into interlayers to expand the interflake spacing and weaken the interaction between MXene layers, which is conducive to further exfoliation and inhibiting the restacking during the assembly process [31, 45]. Typically, Wang et al. [32] developed a simple hydrothermal method to synthesize multilayered Ti₃C₂T_x and investigated the effects of the ratio of reactants, reaction time, and reaction temperature on the product yield. Compared with the direct HF solution etching method, they introduced Ti₃AlC₂ powders into the NH₄F aqueous solution at 150 °C for 12 h. In that process, NH₄F would gradually hydrolyze to produce HF for etching the added powder. Ti₃C₂T_x sheets with a large size (4–15 μm) and defect-free surfaces would be obtained. In addition, a new method with low toxicity and high yield was introduced by Ghidiu et al. [31] to prepare MXene colloidal solution, wherein water was used as the main solvent, HCl, and fluoride salt (LiF in general) as the composite etchant. They first added LiF powders to the HCl solution, followed by the slow addition of Ti₃AlC₂ powders and finally heated in a water bath. Moreover, XRD analysis showed that the layer spacing between sheets in the MXene films produced by a mixed etching agent was larger than that by HF etching, and yields were also higher because of water and/or cations (Li⁺) intercalation in hydrophilic and negatively charged MXene sheets. Additional studies with this compound etching agent demonstrated that the ratio of LiF and sonification treatment (or absence) heavily affect the defect and lateral size of the MXene sheets [46, 47]. Unlike the previously reported method using water as a main solvent, Michel et al. [45] developed a route to fabricate Ti₃C₂T_x MXenes rich in fluorine terminations by etching the MAX phase in a variety of polar solvents with NH₄HF₂ (Fig. 3a, b). Ti₃AlC₂ powders etched by NH₄HF₂ in different organic solvent systems displayed a typical accordion-like morphology, and the TEM micrograph indicates delaminated Ti₃C₂T_x flakes after sonification, confirming the successful synthesis of Ti₃C₂T_x (Fig. 3c, d). The d-spacing of the obtained MXenes was also significantly larger than that of samples etched in an NH₄HF₂ aqueous solution because of the intercalation of NH₄⁺/organic solvent molecule complexes [48]. Another interesting trait of these exfoliated Ti₃C₂T_x flakes is the rich distribution of –F terminations [approximately 70% for those produced in propylene carbonate (PC)], which originated from the NH₄HF₂ in a water-absent environment. Other studies have indicated that water plays the key role in inducing degradation of Ti₃C₂T_x and other MXenes [49]. Therefore, the water-free method may be an alternate synthesis technique for MXene to avoid degradation. More importantly, when MXene exfoliated in propylene carbonate was used as an anode of Na-ion battery, nearly double capacity in a PC-containing electrolyte was observed compared with that when MXene etched in water.

MXenes can also be obtained through an element replacement approach in Lewis acid melt salts. For example, Li et al. [20] synthesized Zn-containing MAX phases (Ti₃ZnC₂, Ti₂ZnC, Ti₂ZnN, and V₂ZnC) and further fabricated –Cl terminated MXenes (Ti₃C₂Cl₂ and Ti₂CCl₂) based on this method with original materials of Ti₃AlC₂ and ZnCl₂. In the case of Ti₃ZnC₂, the synthesis mechanism of the Zn-containing MAX phase can be presented by the following reactions:

$${\text{Ti}}_{{3}} {\text{AlC}}_{{2}} { + 1}{\text{.5ZnCl}}_{{2}} {\text{ = Ti}}_{{3}} {\text{ZnC}}_{{2}} { + 0}{\text{.5Zn + AlCl}}_{{3}} \uparrow$$

(8)

$${\text{Ti}}_{{3}} {\text{AlC}}_{{2}} { + 1}{\text{.5ZnCl}}_{{2}} {\text{ = Ti}}_{{3}} {\text{C}}_{{2}} { + 1}{\text{.5Zn + AlCl}}_{{3}} \uparrow$$

(9)

$${\text{Ti}}_{{2}} {\text{C}}_{{3}} {\text{ + Zn = Ti}}_{{3}} {\text{ZnC}}_{{2}}$$

(10)

Coordinately unsaturated Zn²⁺ can act as Lewis acids because of its strong acceptance of –Cl and electrons. Weakly bonded Al atoms in Ti₃AlC₂ can be easily oxidized into Al³⁺ and then further bonded with –Cl to form AlCl₃ [Reaction (9)]. The produced AlCl₃ has a low boiling point (approximately 180 °C), which easily escapes from the original system at high temperature (550 °C). Ti₃ZnC₂ can be formed as in situ reduced Zn atoms intercalated into the Ti₃C₂ layers and fills the A sites of the MAX phase previously occupied by Al atoms [Reaction (10)]. The phase evolution of the reaction product is under the influence of multiple pathways, most notably the different Ti₃AlC₂/ZnCl₂ ratios. Starting with Ti₃ZnC₂, the final products can become Ti₃C₂Cl₂ with an increasing ZnCl₂ ratio in the original materials. Therefore, a two-step formation process is proposed: the generation of Ti₃ZnC₂ and etching in excess ZnCl₂ (Fig. 4a). Similarly, Fashandi et al. [51] fully replaced the Si atomic layers in Ti₃SiC₂ with a noble metal (Au and Ir) using a solid-state diffusion process at high annealing temperature. Moreover, the separation of Si and Au can be achieved via a thermodynamic drive force at an appropriate temperature. The successful synthesis of the new MXene suggests that the exchange mechanism between the A atomic layer in the MAX phase and metal halide may become a common method for the synthesis of unexplored MXenes with functional A-site elements. Similarly, Huang et al. [52] proposed a more general strategy to synthesize MXenes using direct redox coupling between cations in Lewis acid molten salts and element A at high temperatures. This method successfully generalized the Lewis acid melt salts etching strategy to a variety of chloride salts (i.e., ZnCl₂, FeCl₂) and unconventional MAX phases with A elements Si, Zn, and Ga. The exfoliation process can be illustrated in Fig. 4b. In this study, the synthesis of MXene was performed with Ti₃SiC₂ as the precursor and CuCl₂ molten salt as the etchants. The reaction between Ti₃SiC₂ and CuCl₂ at 750 °C involves the following reactions:

$${\text{Ti}}_{{3}} {\text{SiC}}_{{2}} {\text{ + 2CuCl}}_{{2}} \to {\text{Ti}}_{{3}} {\text{C}}_{{2}} {\text{ + SiCl}}_{{4}} \left( {\text{g}} \right) \uparrow {\text{ + 2Cu}}$$

(11)

$${\text{Ti}}_{{3}} {\text{C}}_{{2}} {\text{ + CuCl}}_{{2}} \to {\text{Ti}}_{{3}} {\text{C}}_{{2}} {\text{Cl}}_{{2}} {\text{ + Cu}}$$

(12)

The redox potential of Cu/Cu²⁺ is − 0.43 eV in the molten salt system at 750 °C. Therefore, the ionized Cu²⁺ in the molten salt can easily oxidize the Si atoms to Si⁴⁺, Si^{4 +} eventually forms SiCl₄ gas with –Cl to escape from the Ti₃C₂ sublayer, and Cu²⁺ is reduced to Cu element [Reaction (11)]. After Cu is removed by washing with subsequent ammonium persulfate solution, Ti₃C₂T_x MXene with –Cl and –O as surface groups can be prepared.

Compared with the molten chloride salt etching methods mentioned above, Urbankowski et al. [18] synthesized Ti₄N₃ MXene using molten fluoride salts (KF, LiF, NaF) to remove the Al layers in Ti₄AlN₃ at 550 °C under an argon atmosphere. Further delamination of the multilayered Ti₄N₃T_x via probe sonication produced few-layered and single-layered flakes (Fig. 5). However, there are still some shortcomings in etching the MAX phase in molten salt. First, it is difficult to completely remove the fluoride and other residues. In addition, the key to most molten salt etching systems is atmosphere protection and temperature control. If the temperature is too high or heated directly in the air, the product may have a cubic phase structure [53].

Since it is difficult to use the transition metals Zr and Hf to form the MAX phase, the corresponding MXenes can be obtained from selectively etching a series of non-MAX phases. The non-MAX phase possesses a similar composition to the MAX phase, while its structure is different from the other known MAX phases. Zhou et al. [54] produced high-purity layered Zr₃Al₃C₅ compounds by an in situ reactive pulsed electric current sintering (PECS) process and as a precursor to be exfoliated by HF acid (Fig. 6a). In this process, the relatively weak Al–C bonding units can be easily broken. The following simplified chemical reactions can describe the etching process of Zr₃Al₃C₅:

$${\text{Zr}}_{{3}} {\text{Al}}_{{3}} {\text{C}}_{{5}} {\text{ + HF}} \to {\text{AlF}}_{{3}} {\text{ + CH}}_{{4}} {\text{ + Zr}}_{{3}} {\text{C}}_{{2}}$$

(13)

$${\text{Zr}}_{{3}} {\text{C}}_{{2}} {\text{ + H}}_{{2}} {\text{O}} \to {\text{Zr}}_{{3}} {\text{C}}_{{2}} {\text{(OH)}}_{{2}} {\text{ + H}}_{{2}}$$

(14)

$${\text{Zr}}_{{3}} {\text{C}}_{{2}} {\text{ + HF}} \to {\text{Zr}}_{{3}} {\text{C}}_{{2}} {\text{F}}_{{2}} {\text{ + H}}_{{2}}$$

(15)

SEM and TEM images revealed the accordion-like structure of HF-treated powders and few-layered Zr₃C₂T_z sheets after ultrasonic treatment, respectively (Fig. 6b–f). Hf-containing layered carbide is more difficult to produce a single phase than Zr-containing carbide through chemical etching the ternary composite Hf–Al–C phase because of the strong interfacial bonding between sublayers. The obtained exfoliation products are mainly cubic phases, usually including Hf₃Al₃C₅, Hf₃Al₄C₆, and Hf₂Al₄C₅ mixed phases [55]. Considering the strong interaction between Hf-C and Al-C layers, it is very important to weaken the interfacial adhesion between Hf-C and Al-C sublayers for further exfoliation. Based on the above experiments and analysis, Zhou et al. [56] introduced a small amount of Si into the Al sites and synthesized Hf₂[Al (Si)]₄C₅ and Hf₃[Al (Si)]₄C₆ layered parent compounds by PECS process. With the solid solution as the precursor and HF acid as the etching agent, selective exfoliation of the Al(Si)–C structural unit was demonstrated, producing 2D Hf-containing MXenes for the first time (Fig. 7a). The etching mechanism is shown in Table 1 [56]. The representative SEM and TEM images demonstrated the successful etching and exfoliation process (Fig. 7b–e).

Table 1 Chemical equations for etching behaviors and corresponding adhesive energies (in eV/Å²)

Full size table

To explore the exfoliation mechanism by means of the binding energy and atomic charge calculation, the microscopic mechanism of Si do** facilitating the process of hydrofluoric acid exfoliation was clarified. Since Si has one more valence electron than Al, Al can effectively reduce the interface binding energy between the Hf atomic layer and the exfoliated Al (Si)₄C₄ layer from 8.60 to 4.05 eV. Therefore, the introduction of Si has realized the effective tuning of the Hf–C and Al (Si)–C lamellar interface within the unit cell, significantly weakening the interface bonding and introducing efficient exfoliation.

Given that current synthesis methods mainly involve a highly concentrated HF solution or a mixture of fluoride and strong acids for etching the A atomic layers in MAX phases, the produced MXene sheets were normally accompanied by large amounts of –F terminal groups. Although the methods are effective, these processes are environmentally harmful and decrease the material performance (for example, capacitance) because of the chemical inert –F terminals. Several novel studies have revealed that MXenes can also be produced without fluoride by etching their parent MAX phases. Based on the Bayer process, Li et al. [37] proposed a fluorine-free method for etching of the Al element in Ti₃AlC₂ via hydrothermal treatment in 27.5 mol/L NaOH (Fig. 8a). The entire process was totally free of fluorine, yielding –OH and –O terminated multilayer Ti₃C₂T_x sheets with nearly 92 wt% purity. Moreover, they systematically investigated the effects of temperature and alkali concentration on the etching results. The results showed that the high temperature could accelerate the formation of Ti₃C₂ because the reaction between alkali and undissolved Al hydroxides (Al(OH)₃) is an endothermic process, and the purities of the resulting MXenes are dominated by the alkali concentration. Importantly, the fabricated NaOH–Ti₃C₂T_x thin-film electrode without –F terminal groups (thickness 52 μm, density 1.63 g/cm³) delivered a high gravimetric capacitance value of 314 F/g at 2 mV/s or 254 F/g at 1 A/g, superior to that of HF–Ti₃C₂T_x (100 F/g at 2 mV/s, terminated with –O, –OH, and –F). Similarly, Pang et al. [57] developed an HF-free strategy for synthesizing multiple kinds of MXenes (Ti₂CT_x, Cr₂CT_x, and V₂CT_x) based on a thermally assisted electrochemical etching method. In this paper, we will elucidate the novel process by examining a Ti₂CT_x example in diluted HCl acid. By adopting carbon fiber cloth and carbon black additives to Ti₂AlC powder to produce a composite electrode, the small voltage (0.3 V vs. RHE is the best) and mild heating caused effective electrochemical etching process. Moreover, the as-synthesized MXene via the HF-free strategy reached 25 μm and a flower-like architecture with a rougher surface than the unetched Ti₂AlC. Such a morphological change indicates effective electrochemical-etching, particularly for the case with a thermal effect.

Excellent properties of 2D materials are only revealed after being delaminated into single or a few atomic layer thicknesses; as a result, the exfoliation process is very important in the preparation of 2D MXene materials [58]. Even after being etched, large amounts of MXene sheets are still restacked because of the presence of hydrogen bonds and electronic attraction [59]. Therefore, the yield of single/few-layered MXene sheets obtained by simple mechanical delamination is relatively low, and delaminated MXene sheets are easy to be oxidized and degraded. Therefore, the subsequent intercalation and delamination process after etching is of significant importance for obtaining single- or few-layered MXene sheets with larger sizes and fewer defects. The post-etched powders are covered with functional groups (–OH, –F, –O, etc.), so MXene flakes are electronegative. Some cations (Li⁺, Na⁺, H⁺, etc.) and/or polar organic molecules (dimethyl sulfoxide (DMSO), N-butyl amine, etc.) can spontaneously intercalate between interlayers because of electrostatic attraction, which is conducive to expanding the interlayer spacing and accelerating the exfoliation of etched samples. Furthermore, the introduction of these guest molecules/ions will also inhibit restacking when exfoliated MXene flakes are further assembled into a film [60,61,62]. DMSO was effective in delaminating Ti₃C₂T_x MXene while it was not suited for other MXenes [63]. The single- and few-layered 2D Ti₃C₂T_x sheets are generally prepared through the mixture of HF etched powder in a DMSO solution for intercalating the organic compound into the layered structure, and sonication in water under argon atmosphere for delamination. Gogotsi et al. [64] obtained individual 2D Nb₂CT_x sheets via an amine-assisted delamination process and successfully inserted isopropylamine into Nb₂CT_x layers. The schematic of the delamination strategy is shown in Fig. 8b. Isopropylamine is proposed to produce R-NH₃⁺ after dissolving in water, and will intercalate into the Nb₂CT_x layers via the electrostatic attraction. In addition, isopropylamine has a three-carbon-atom alkyl tail, which may be small enough to overcome the spatial hindrance of intercalation, and large enough to push the MXene layer away. This approach seems to be more general and has the potential to delaminate Ti₃C₂T_x, Nb₄C₃T_x, and other MXenes.

In addition to the above-mentioned synthesis methods (or top-down methods), MXenes can also be produced by bottom-up methods such as atomic layer deposition (ALD) and chemical vapor deposition (CVD). Halim et al. [48] reported the successful deposition of Ti₃AlC₂ thin films from three elemental targets (Ti, Al, C) through direct current magnetron sputtering (DCMC). Using NH₄HF₂ as etchants, the continuous epitaxial Ti₃C₂ thin films could be obtained by selectively removing Al layers, and NH₃ and NH₄⁺ were successfully intercalated Ti₃C₂T_x interlayers. A 1 cm × 1 cm thin film (∼ 19 nm) exhibited ∼ 90% light transmittance in the visible-to-infrared range, with a metallic-like nature of the conductivities. CVD can be used to directly synthesize ultrathin MXene material, which is a relatively new method for fabricating MXene-based materials. For example, Xu et al. [33] successfully fabricated 2D ultrathin Mo₂C crystals through a CVD process with a temperature higher than 1085 °C; however, such bottom-up synthesis methods are rarely reported on other MXenes because of the possible bond energies. In this study, methane was used as the carbon source, and a Cu foil sitting on a Mo foil was used as the substrate. The synthesized high-quality 2D ultrathin Mo₂C crystals can reach lateral sizes greater than 100 μm with a few nanometers in thickness. More importantly, the size and thickness of the crystals can be well tuned by varying the experimental conditions, wherein the nucleation density and lateral size can increase with the growing temperature and growing time, respectively.

Although numerous methods have been developed to fabricate various types of MXenes, the current techniques are still restricted by many disadvantages, such as time consumption, heavy pollution, high cost, low yields even on a laboratory scale, low quality, and poor stability. Therefore, the scalable and cost-effective synthesis methods for high-quality MXenes still need to be explored. To realize these goals, attention should be devoted to environmentally friendly etchants and abundantly available inexpensive raw materials. The time of fabrication and yield are also worth considering; as a result, there is a need to focus on fast and easy ways for high yields.

Assembly Technologies of MXene Films

MXenes and their composites have been widely researched in various fields as different forms such as powders [41], films [11], and hydrogels [65]. However, given the increased number of published papers, MXene is still generally assembled into films. For example, MXene films can be applied as flexible electrodes [42, 66], membrane separation (including liquid separation membranes and gas separation membranes) [67, 68], battery separators [112,113], which play an important role in our daily life with their long cycle life, charging/discharging rates, and high energy density. Supercapacitors comprised of novel electrode materials have caused widespread attention in recent years and are thought to affect the development of next-generation electronic devices well. MXene films are attractive as advanced electrodes in supercapacitors given their high electric conductivity, excellent mechanical property, and Faraday pseudocapacitive charge storage mechanism [114, 14e, f). The excellent electrochemical performance is ascribed to the large amount of fluorine terminations on the MXene surfaces, which can form a uniform and dense solid electrolyte interface with LiF and effectively optimize the electromigration of lithium ions.

Sodium-ion batteries are another essential energy storage device because of their security and low-cost. In addition, Ti₃C₂ sheets with –F, –O, and –OH terminations are approximately 0.19, 0.2 and 0.013 eV on Na⁺ diffusion barriers, respectively, demonstrating superior Na⁺ diffusion kinetics and great application potential in sodium-ion batteries [139]. Zhao et al. [140] synthesized molecular-level coupling PDDA-BP/Ti₃C₂ heterostructures via an electrostatic attraction self-assembly strategy, which play to the advantages of the high capacity of black phosphorene (BP) and excellent electronic conductivity of Ti₃C₂. The freestanding films exhibited an ultra-high reversible capacity (1112 mA·h/g) after 500 cycles and showed excellent cycling stability. In addition, DFT calculations were performed to reveal the underlying mechanism of the sodiation and relaxation process when adding Na on top of the surface functional groups (such as –F, –O, and –OH). The simulation results manifest that the enhanced sodium storage performance and resultant ultra-high reversible capacity may be ascribed to the fast ion diffusion and charge transfer kinetics originating from the mixed absorption and decreased binding energy. By processing the various 2D MXene flakes (V₂CT_x, Ti₃C₂T_x, and Mo₂CT_x) onto hollow spheres (PMMA), respectively, and further forming 3D architectures via a sacrificial template approach, freestanding, flexible, and highly conductive 3D macroporous MXene films were successfully fabricated [148]. Therefore, MXene membranes have attracted attention in water purification and have been proved to possess extraordinary permeation properties. Ren et al. [149] pioneered the use of MXene membranes to realize charge- and size- selective rejection of ions and molecules, studying the correlation between water flux and membrane thickness. The micrometer-thick Ti₃C₂T_x membranes possessed ultrafast water permeation (37.4 L/(bar h m²)) as well as attractive separation property toward single-, double-, triple-charged metal cations and dye cations with varying sizes. The ions with radii larger than the interlayer distance demonstrated a low permeation rate (∼ 7 × 10⁻⁴ mol/(hm²) because they did not pass through the Ti₃C₂T_x membrane. Moreover, by electrically modulating the surface charge of Ti₃C₂T_x with an applied voltage (electrochemical filtration), the ion sieving process can be further enhanced. In addition, Wang et al. [67] successfully prepared a 2D lamellar membrane with ultrashort transport pathways and abundant nanochannels using simple filtration. The positively charged Fe(OH)₃ colloidal solution was used as a pore former to create expanded channels through intercalating layers of negatively charged MXene flakes. This MXene membrane could reject particles with a diameter larger than 2.5 nm in water (> 90%) and still maintain high water permeation and excellent stability (more than 1000 L/(m² hbar) after continuously operating for 24 h. Subsequently, an Al³⁺ intercalated and non-swelling MXene membrane was prepared via a simple “concentration diffusion” method. Al³⁺ played a crucial role in firmly fixing the MXene layers through the interaction with oxygen-containing terminal groups on the MXene surfaces and provided Al³⁺-intercalated MXene membranes an opportunity to withstand the high driving force induced in a high salt concentration. Compared with pristine MXene membranes without any treatment, the Al³⁺-intercalated MXene membrane effectively inhibited the swelling in the aqueous solution. The ion-intercalated membrane showed both a high salt rejection rate (NaCl, 99.5%) and improved water flux (2.81 L/(m² h)) [150].

Additionally, ** profiles of the pixel signals. Reproduced with permission [177]. Copyright 2020, American Chemical Society. d Design and assembly of piezoresistive sensors with bionic spinous microstructure.

Full size image

Given that MXene films and their composite films possess peculiar physical (metallic conductivity, layered structure), chemical (abundant surface groups), and biological properties (hydrophilicity), some parameters associated with these properties may occur subtle deviation as external conditions changes. Therefore, MXene-based films can also work as sensors to detect the change of external conditions [34]. Various sensing platforms based on MXenes have been fabricated to quantitatively detect external stimuli, including pressures, ion/gases, sounds, and human activities. Stacking properties between MXene flakes can be altered by external strain changes, which in turn can change the interflake resistance of the devices. Therefore, this property can also be utilized to fabricate highly sensitive MXene-based piezoresistive sensors for detecting slight movements of humans. An et al. [176] illustrated that Ti₃C₂/PDAC films could be used as a strain sensor, which can sense object deformations according to the resistance change during the deformation process. Compared with traditional graphene- or carbon nanotube-based sensors for electronic devices, the Ti₃C₂/PDAC membrane-based sensor was more suitable for a variety of complex deformation modes while maintaining outstanding electronic conductivity. Li et al. [177] prepared hydrophobic organic/inorganic composite films using natural poly(vinylidene fluoride) trifluoroethylene (P(VDF-TrFE)) and multilayer Ti₃C₂T_x via a spin-coating method, and then fabricated stable piezoresistive pressure sensors (Fig. 17c). In addition, a MXene-based piezoresistive sensor with a randomly distributed spinous microstructure was reported that was designed and manufactured by a facile abrasive paper stencil printing process. This sensor was ultrathin, flexible, and highly sensitive, and therefore easy to attach to the skin for detecting human activities and human–computer interaction (Fig. 17d) [178]. MXenes films can also be utilized for detecting various gases and biologically important molecule because of the active surface functional groups and layered structures. Ti₃C₂T_x chemical sensors with superior sensing properties for volatile organic compounds (VOCs) (ammonia, acetone, ethanol, and propanol) in ultralow detection limits (50–100 ppb) have been synthesized [179]. This sensor manifested high selectivity toward hydrogen-bonding gases over acidic gases. Moreover, given the Ti₃C₂T_x is fully covered with active surface terminations, selectivity toward various gases may also be adjusted by ligand functionalization or defect control. For example, Ti₃C₂T_x sensors via surface treatment with fluoroalkylsilane (FOTS) molecules provide a superhydrophobic surface, mechanical/environmental stability, and enhanced sensing performance for oxygen-containing VOCs (acetone, ethanol, and 2-propanol) [180].

MXene-based films are promising alternatives to traditional 2D films widely used in application fields mentioned above because of the various functionalities of MXenes. While the emerging MXene nanomaterials are promising in the design of performance films, numerous challenges still restrict the commercialization of current MXene-film based devices. For example, MXene-based films are not cost-competitive and are difficult to scale-up despite the improved performances compared with commercial devices. Improved etching methods and novel assemblies can be used to further investigate and solve these problems. Additionally, a reasonable design of MXene-film based devices should be further explored and promoted, especially in energy-storage devices and flexible electronics. The relationship between property and structure in the MXene-based films need to be further investigated by theoretical simulation and experiment, which is an important step for in-depth research of the nature of MXenes to broaden their application fields.

Conclusion and Outlook

In summary, we focused on the synthesis methods, assembly technologies, and intriguing applications of MXene-based films. The practical applications of MXene films have been summarized in detail, including electrochemical energy storage, EMI shielding, membrane separation, and other emerging applications. MXene sheets and composite films have gained remarkable achievements in various applications. Nevertheless, the development of MXene film is still in its infancy, and there are still many urgent problems that remain to be addressed before the practical application of these materials.

Even if the synthesis of various MXenes is feasible by theoretical calculation, the practical fabrication is still limited by the difficulty of synthesizing the corresponding MAX phases and instability of MXenes after exfoliation. Therefore, new exfoliation and synthesis methods of new precursors are urgent problem. Green and mild synthetic approaches are necessary for fabricating MXenes with high yield and high quality. Additionally, we can devote vast attention to the new-style MAX phases with various elements (not only conventional Al) to expand the MAX family.

Similar to other 2D nanomaterials, morphological improvements and surface modifications have a significant impact on increasing the number of active sites. This is very important for the production of high quality MXenes with large-scale sheets and nano-scale defects for application to high-performance batteries or capacitors. For lithium-ion batteries and sodium-ion batteries, if the electrode material has no defects or functional groups, it will greatly reduce the initial Coulombic efficiency. In addition, a higher specific surface area and pore volume can be effectively produced by controlling the porosity and curvature of the MXene layer; the addition of specific groups has a promoting effect on both aspects.

Although MXenes have achieved outstanding performance in many applications, especially in the field of electrochemistry, their physical mechanisms need to be further studied. The restacking tendency of MXene sheets may not be satisfactory in realizing its actual electrochemical performance, which can result in adverse effects on the commercial production of MXene-film based devices. For example, when MXene film is fabricated by a simpler VAF method, if the nanosheets are self-stacking, the electrochemical performance will decrease from the reduced transmission of ions. Therefore, an in-depth study of the restacking mechanism is necessary. In addition, the combination of a hydrophilic surface and excellent electrical conductivity enables multifunctional design and excellent processing performance of MXenes, which provides new opportunities for exploring unknown fields and introduce a new pathway to the advancement in various applications. Another promising prospect is to convert MXene to commercial products [181]. To meet the requirements of industrial application, the technical issues for mass production and process integration should be considered. Therefore, it is necessary to well understand the exfoliation mechanism of the MAX phase from the most basic structure and investigate the mechanism of the fundamental properties and functionality of MXenes to scale-up the production process in a low-cost and environmentally friendly way.

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Acknowledgements

This work was supported by the National Natural Science Foundation of China (21878062), the Natural Science Foundation of Heilongjiang Province for Distinguished Young Scholars (JQ2020B001) and State Key Laboratory of Urban Water Resource and Environment (Harbin Institute of Technology) (No. 2020DX02).

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MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, State Key Laboratory of Urban Water Resource and Environment (SKLUWRE), School of Chemistry and Chemical Engineering, Harbin Institute of Technology, Harbin, 150000, China
**aohua Li, Feitian Ran, Fan Yang, Jun Long & Lu Shao

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**aohua Li
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Feitian Ran
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Fan Yang
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Jun Long
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Lu Shao
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Correspondence to Lu Shao.

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Li, X., Ran, F., Yang, F. et al. Advances in MXene Films: Synthesis, Assembly, and Applications. Trans. Tian** Univ. 27, 217–247 (2021). https://doi.org/10.1007/s12209-021-00282-y

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Received: 16 December 2020
Revised: 01 January 2021
Accepted: 19 January 2021
Published: 07 March 2021
Issue Date: June 2021
DOI: https://doi.org/10.1007/s12209-021-00282-y

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Advances in MXene Films: Synthesis, Assembly, and Applications

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