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Guidelines for Synthesis and Processing of Two-Dimensional Methods/Protocols pubs.acs.org/cm Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene) Mohamed Alhabeb, Kathleen Maleski, Babak Anasori, Pavel Lelyukh, Leah Clark, Saleesha Sin, and Yury Gogotsi* A.J. Drexel Nanomaterials Institute and Department of Materials Science and Engineering, Drexel University, 3141 Chestnut Street, Philadelphia, Pennsylvania 19104, United States *S Supporting Information ABSTRACT: Two-dimensional (2D) transition metal carbides, carbonitrides, and nitrides (MXenes) were discovered in 2011. Since the original discovery, more than 20 different compositions have been synthesized by the selective etching of MAX phase and other precursors and many more theoretically predicted. They offer a variety of different properties, making the family promising candidates in a wide range of applications, such as energy storage, electromagnetic interference shielding, water purification, electrocatalysis, and medicine. These solution-processable materials have the potential to be highly scalable, deposited by spin, spray, or dip coating, painted or printed, or fabricated in a variety of ways. Due to this promise, the amount of research on MXenes has been increasing, and methods of synthesis and processing are expanding quickly. The fast evolution of the material can also be noticed in the wide range of synthesis and processing protocols that determine the yield of delamination, as well as the quality of the 2D flakes produced. Here we describe the experimental methods and best practices we use to synthesize the ff ff most studied MXene, titanium carbide (Ti3C2Tx), using di erent etchants and delamination methods. We also explain e ects of synthesis parameters on the size and quality of Ti3C2Tx and suggest the optimal processes for the desired application. ■ INTRODUCTION mechanical exfoliation hardly possible. To date, more than Since the isolation of single layer graphene in 2004,1 20 members of the MXene family have been synthesized, and dozens more are predicted, making it one of the fastest growing two-dimensional (2D) materials have gained tremendous atten- 7 tion because of their distinctive properties relative to their bulk 2D material families. Additionally, the MXene family comes in form. The isolation of graphene has become a reference for all three atomic structures, ranging from M2XtoM3X2 and M4X3, yielding tunability and opportunity to discover and mold materials 2D materials and opened the possibility to discover even more. 7,10,11 Today, there are dozens of new 2D materials, including hexag- based on necessary demands. In contrast to most other 2D materials, including graphene, onal boron nitride, transition metal dichalcogenides, transition 7 metal oxides, clays, etc.2 MXenes possess hydrophilic surfaces and high metallic conductivities (∼6000−8000 S/cm),12,13 showing promising − Downloaded via NORTH DAKOTA STATE UNIV on October 8, 2018 at 18:08:40 (UTC). In 2011, a new family of 2D materials, named MXenes, were 14 17 3 performance in energy storage devices, water desalina- discovered by Drexel University scientists. The MXene family 18 19 20 See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles. is comprised of transition metal carbides, carbonitrides, and tion, catalysis, electromagnetic interference shielding, transparent, conducting thin films,12,21,22 and many other nitrides with a general formula of Mn+1Xn, where M represents 7 transition metals (such as Sc, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, applications. 3,4 “ ” Since their discovery, production of multilayered MXene etc.) and X is carbon and/or nitrogen. The name MXene fl was given to describe the similarities between this 2D material akes was possible through wet-chemical etching with HF, and different MXene compositions were synthesized in this form, family and graphene but also to recognize the parent ternary 3,23,24 such as Ti2CTx,Ti3CNTx,Nb2CTx,andV2CTx (Figure 1). carbide and nitrides, MAX phases, which MXenes are fl synthesized from.5 MAX phases are layered ternary carbides However, it was not until 2013 when single-layer MXene akes were isolated by intercalating large organic molecules and and nitrides with a general formula Mn+1AXn, where A delaminating the sheets from each other, opening the door to represents elements from the group 13 and 14 of the periodic 25 table.5,6 exploration of the truly 2D nature of MXenes. In 2014, MXenes reported to date are synthesized by wet-chemical Ti3C2Tx MXene was produced using a HF-containing etchant fl 21 etching in hydrofluoricacid(HF)orHF-containingor such as ammonium bi uoride (NH4HF2) salt, and later in the − HF-forming etchants,7 9 which add surface functionalities − − − such as O, F, or OH, represented by Tx in this formula Received: July 8, 2017 as Mn+1XnTx. Etching is required because of strong chemical Revised: August 25, 2017 bonds between A and M elements in MAX phases that make Published: August 25, 2017 © 2017 American Chemical Society 7633 DOI: 10.1021/acs.chemmater.7b02847 Chem. Mater. 2017, 29, 7633−7644 Chemistry of Materials Methods/Protocols fi Figure 1. Timeline of MXene: a journey from 2011 to now. In 2011, the rst MXene multilayered powder (Ti3C2Tx) was made by selective etching fl 3 ff of Al from Ti3AlC2 using HF acid. A schematic of Ti3C2Tx ake structure is shown as an example. In 2012, a variety of di erent MXenes, such as Ti2CTx, (Ti,Nb)2CTx, (V,Cr)3C2Tx,Ti3CNTx, and Ta4C3Tx, were also synthesized, and MXenes became a family of transition metal carbides and carbonitrides.21 In 2013, single layers of MXenes were isolated by intercalation and delamination with organic molecules.23 In 2014, in situ HF 24 15 etchants such as NH4HF2 or LiF/HCl mixtures were used. The latter resulted in Ti3C2Tx with clay-like behavior and is called the clay method. fl 15 With sonication of Ti3C2Tx clay in water, submicrometer lateral-size single akes of Ti3C2Tx were isolated. In 2015, large scale (high yield) delamination of different MXenes using the amine-assisted method or TBAOH were reported.25,26 Additionally, two subfamilies of MXenes, ff ff ordered-double-transition metal carbides, where two di erent transition metals occupy di erent atomic layers, were discovered (such as Mo2TiC2Tx, ff 27 fl Cr2TiC2Tx,Mo2Ti2C3Tx), adding more than 25 di erent possible MXenes to the family. In 2016, delamination and isolation of large single akes μ of Ti3C2Tx (>2 m) were achieved without sonication through optimization of the LiF/HCl etching method. The optimized method is referred to as fl 28 MILD, making single- ake characterization possible. In 2017, by synthesizing in-plane double transition metal MAX phase ((Mo2/3Sc1/3)2AlC) and 8 etching one of the transition metals, MXene with ordered divacancies (Mo1.3CTx) was synthesized. SEM images in 2014 and 2016 show Ti3C2Tx flakes on an alumina membrane. Scale bars are 2 μm. “ ” same year, Ti3C2Tx clay was synthesized by taking advantage etch aluminum (Al) out of Ti3AlC2 with concentrated HF of making in situ HF through addition of lithium fluoride (LiF) (∼50 wt %) at room temperature.25 Based on the type of salt to hydrochloric acid (HCl), significantly simplifying the MXene and the synthesis conditions, the intercalants may vary synthesis method and improving MXene performance in energy as well as the delamination yield.7 We recently summarized storage applications (Figure 1).15 With the need for methods to etching and delamination conditions reported in literature for increase the delamination yield, in 2015 additional organic most MXenes known to date, and we encourage the readers to intercalants were used, such as isopropylamine26 and tetra- view the referenced review on etching, delamination, and 27 7 butylammonium hydroxide (TBAOH). Moreover, in 2015, processing protocols for MXenes besides Ti3C2Tx. two new MXene subfamilies, ordered double-transition metal Here, we discuss the best practices used in our lab and ′ ″ ′ ″ ′ ″ MXenes, M 2M C2, and M 2M 2C3, where M and M are two provide step-by-step guidance for room temperature synthesis different early transition metals, were discovered, further expand- of titanium carbide (Ti3C2Tx), the most studied and widely ing the 2D family.28 Each of these evolutionary discoveries has used MXene. We categorize currently used etchants for added tunability and diversity to MXene family. selective removal of Al from Ti3AlC2 structure into two fl In 2016, larger single Ti3C2Tx akes were isolated by using types: synthesis protocols using HF and protocols using in situ the minimally intensive layer delamination (MILD) meth- formed HF. Moreover, we provide a guideline on how to od,20,29 where manual shaking (no sonication) was used and delaminate as-synthesized materials into colloidal solutions resulted in larger and less defective single flakes of MXene.13 even without sonication. We also discuss storage, processing, The MILD method expanded the opportunities for research and deposition techniques to make different types of con- fi on electronic, optical, and size-dependent material properties ductive Ti3C2Tx MXene lms. as well as further enhanced the scalability and production of ■ DISCUSSION OF METHODS Ti3C2Tx MXene. A timeline progress of MXenes is shown in Figure 1. There are many different protocols for synthesizing MXene The exact synthesis conditions used to produce MXenes materials reported in literature,7 and one synthesis route may influence the resulting properties and thus are directly related be better for one application but not suitable for another
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