Synthesis of two-dimensional Ti3C2Tx MXene using HCl+LiF etchant: Enhanced exfoliation and delamination

Zhang, Tian; Pan, Limei; Tang, Huan; Du, Fei; Guo, Yanhua; Qiu, Tai; Yang, Jian

doi:10.1016/j.jallcom.2016.10.127

Cited by 372 publications

(175 citation statements)

References 36 publications

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“…At most voltages, aqueous EPD films had c lattice parameters (c-LP) of 22-23 Å, whereas values ranging from 25-30 Å have been reported in literature for Ti 3 C 2 T x films made by other methods from aqueous suspensions. 30,34,46 The reasons for the lower c-LP of these EPD-processed films and asymmetry in the shape of the (002) basal peaks are not clear at this time but could be the result of water being forced out from between the flakes as they come together to form a deposit.…”

Section: Resultsmentioning

confidence: 95%

“…Under a very simplistic model, applying the Smoluchowski equation and assuming spherical particles, approximate zeta potentials can be estimated of −58 ± 3 mV and −61 ± 3 mV, for water and PC respectively, in agreement with previously reported measurements on colloidal Ti 3 C 2 T x suspensions. 45,46 General film characteristics.-At first, EPD from aqueous suspensions was performed under constant-voltage conditions at 5, 10, 15, 20 and 25 V for 600 s each. Initially, the deposition current decreased exponentially for all voltages.…”

Section: Resultsmentioning

confidence: 99%

See 1 more Smart Citation

Electrophoretic Deposition of Two-Dimensional Titanium Carbide (MXene) Thick Films

Collini

Kota

Dillon

et al. 2017

J. Electrochem. Soc.

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Herein, we demonstrate the fabrication of Ti 3 C 2 T x MXene films using electrophoretic deposition (EPD). A systematic study under constant voltage conditions from aqueous and propylene carbonate-based suspensions was performed to investigate the effects of the EPD process parameters on film morphology, flake orientation, and functional properties. From measured suspension properties, the kinetics of deposition from both suspension media were successfully described by the well-established Sarkar model of EPD. Remarkably, EPD-processed films have electrical conductivities of 7400 S/cm, on par with the highest values reported in the literature for Ti 3 C 2 T x MXene. When employed as electrochemical capacitor electrodes in 1 M H 2 SO 4 , the capacitances were comparable to literature values. Given the process scalability and the morphological control that is possible, these results bode well for EPD as a fast, high-throughput method for making MXene films. Electrophoretic deposition (EPD) is a process wherein an electric field is applied to a stable colloidal suspension in between two electrodes.1 As a consequence, two distinct processes occur, as shown in Figure 1a: (1) charged particles in the colloid move toward the electrode of opposite polarity to that of the particles' surface charge (electrophoresis) and, (2) a solid deposit is formed by coagulation at the suspension-electrode interface (deposition). This technique is well-studied and successfully implemented for high-throughput production of dense, void-free ceramic structures ranging from thin coatings to bulk layers several centimeters thick.2 Because of the flexibility and scalability of the deposition apparatus (e.g. power sources and size/shape of deposition electrodes and cell), fast deposition rates, and excellent microstructural control compared to other processing methods, EPD has been used for commercial-scale production of various engineering and traditional ceramics. [2][3][4] In recent years, EPD has also become a versatile technique for making monolithic films and nanocomposites of two-dimensional (2D) materials -such as graphene, transition metal dichalcogenides, and layered transition metal oxides 5-10 -due to advances in colloidal processing. Recently, we discovered a new family of two-dimensional (2D) early transition metal carbides and nitrides, that we labeled MXene, because they are derived from the MAX phases and share properties similar to graphene. 11,12 The MAX phase composition is M n+1 AX n , where M is an early transition metal, A is an A-group element (mostly group 13 and 14 elements), X is carbon and/or nitrogen, and n = 1 to 3. The exfoliation process is carried out by selectively etching away the 'A' layers by hydrofluoric acid (HF) alone or by hydrochloric acid (HCl) combined with pre-dissolved fluoride salts. [13][14][15][16] The resulting material consists of loosely bonded layers of M n+1 X n T x , where T represents surface functionalization by -OH, -F and/or -O groups, [17][18][19] that can subsequently be delaminated...

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Section: Resultsmentioning

confidence: 95%

Section: Resultsmentioning

confidence: 99%

Electrophoretic Deposition of Two-Dimensional Titanium Carbide (MXene) Thick Films

Collini

Kota

Dillon

et al. 2017

J. Electrochem. Soc.

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“…Considering the hazardous nature of hydrofluoric acid, a mild etchant mixed solution made of lithium fluoride (LiF) and hydrochloric acid (HCl) was developed for the in situ formation of hydrofluoric acid (HF) to achieve selective etching . Typically, LiF powder is added to HCl solution under stirring at room temperature until a clear solution is formed, which yields HF with a low concentration (3–5%) according to the following equation:

LiF (aq) + HCl (aq) = HF (aq) + LiCl (aq)

…”

Section: Mxenes Synthesismentioning

confidence: 99%

Two‐Dimensional Transition Metal Carbides and Nitrides (MXenes): Synthesis, Properties, and Electrochemical Energy Storage Applications

Zhang

et al. 2019

Energy & Environ Materials

416

181

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A family of 2D transition metal carbides and nitrides known as MXenes has received increasing attention since the discovery of Ti3C2 in 2011. To date, about 30 different MXenes with well‐defined structures and properties have been synthesized, and many more are theoretically predicted to exist. Due to the numerous assets including excellent mechanical properties, metallic conductivity, unique in‐plane anisotropic structure, tunable band gap, and so on, MXenes rapidly positioned themselves at the forefront of the 2D materials world and have found numerous promising applications. Particular interest is devoted to applications in electrochemical energy storage, whereby 2D MXenes work either as electrodes, additives, separators, or hosts. This review summarizes recent advances in the synthesis, fundamental properties and composites of MXene and highlights the state‐of‐the‐art electrochemical performance of MXene‐based electrodes/devices. The progresses in the field of supercapacitors and Li‐ion batteries, Li‐S batteries, Na‐ and other alkali metal ion batteries are reviewed, and current challenges and new opportunities for MXenes in this surging energy storage field are presented. In the focus of interest is the possibility to boost device‐level performance, particularly that of rechargeable batteries, which are of utmost importance in future energy technologies. Very recently, the 2019 Nobel Prize in Chemistry was awarded to the inventors of the Li‐ion battery. For sure, this will provide an additional stimulation to study fundamental aspects of electrochemical energy storage.

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“…Since their discovery, MXenes have been intensely and extensively studied as regards their synthesis, properties, and applications . MXenes are synthesized by selectively etching layers of “A” elements from the homologous three‐dimensional (3D) MAX phases, and the frequently used etchant is HF, NH 4 HF 2 , and so on . MAX phases are a family of stratified tribasic metal carbides, nitrides, and carbonitrides.…”

Section: Introductionmentioning

confidence: 99%

“…[8][9][10] MXenesare synthesized by selectively etchingl ayers of "A" elements from the homologous three-dimensional( 3D) MAX phases,a nd the frequently used etchant is HF,N H 4 HF 2 ,a nd so on. [11][12][13][14][15] MAX phases are af amily of stratified tribasic metal carbides, nitrides, and carbonitrides. They are typicallyd enoted by the formula M n + 1 AX n (n = 1, 2, 3), in which M, A, and X stand for early d-block transition metals, main-group sp elements (prevailingly III Ao rI VA), and both Ca nd Na toms,r espectively.…”

Section: Introductionmentioning

confidence: 99%

Functional MXene Materials: Progress of Their Applications

Wang

Cao

et al. 2018

Chemistry An Asian Journal

192

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Nowadays, two-dimensional materials have many applications in materials science. As a novel two-dimensional layered material, MXene possesses distinct structural, electronic, and chemical properties; thus, it has potential applications in many fields, including battery electrodes, energy storage materials, sensors, and catalysts. Up to now, more than 70 MAX phases have been reported. However, in contrast to the variety of MAX phases, the existing MXene family merely includes Ti C, Ti C , (Ti , Nb ) C, (V , Cr ) C , Nb C, Ti CN, Ta C , V C, and Nb C . Among these materials, the Ti C T MXene exhibits prominently high volumetric capacitance, and the rate at which it transports electron is suitable for electrode materials in batteries and supercapacitors. Hence, Ti C T is commonly utilized as an electrode material in ion batteries such as Li , Na , K , Mg , Ca , and Al batteries. What is more, Ti C has the biggest specific surface area among all of these potential MXene phases, and therefore, Ti C has remarkably high gravimetric hydrogen storage capacities. In addition, Ti CO materials display extremely high activity for CO oxidation, which makes it possible to design catalysts for CO oxidation at low temperatures. Furthermore, Ti C T with O, OH, and/or F terminations can be used for water purification owing to excellent water permeance, favorable filtration ability, and long-time operation ability. This review supplies a relatively comprehensive summary of various applications of MXenes over the past few years.

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Synthesis of two-dimensional Ti3C2Tx MXene using HCl+LiF etchant: Enhanced exfoliation and delamination

Cited by 372 publications

References 36 publications

Electrophoretic Deposition of Two-Dimensional Titanium Carbide (MXene) Thick Films

Electrophoretic Deposition of Two-Dimensional Titanium Carbide (MXene) Thick Films

Two‐Dimensional Transition Metal Carbides and Nitrides (MXenes): Synthesis, Properties, and Electrochemical Energy Storage Applications

Functional MXene Materials: Progress of Their Applications

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