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Title: Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti 3C 2T x MXene) [Guidelines for Synthesis and Processing of 2D Titanium Carbide (Ti 3C 2T x MXene)]

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. Furthermore we describe the experimental methods and best practices we use to synthesize the most studied MXene, titanium carbide (Ti 3C 2T x), using different etchants and delamination methods. We also explain effects of synthesis parameters on the size and quality of Ti 3C 2T xmore » and suggest the optimal processes for the desired application.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1];  [1];  [1];  [1]; ORCiD logo [1]
  1. Drexel Univ., Philadelphia, PA (United States). A.J. Drexel Nanomaterials Institute and Department of Materials Science and Engineering
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1399240
Grant/Contract Number:
AC05-00OR22725
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 29; Journal Issue: 18; Journal ID: ISSN 0897-4756
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Alhabeb, Mohamed, Maleski, Kathleen, Anasori, Babak, Lelyukh, Pavel, Clark, Leah, Sin, Saleesha, and Gogotsi, Yury G. Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene) [Guidelines for Synthesis and Processing of 2D Titanium Carbide (Ti3C2Tx MXene)]. United States: N. p., 2017. Web. doi:10.1021/acs.chemmater.7b02847.
Alhabeb, Mohamed, Maleski, Kathleen, Anasori, Babak, Lelyukh, Pavel, Clark, Leah, Sin, Saleesha, & Gogotsi, Yury G. Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene) [Guidelines for Synthesis and Processing of 2D Titanium Carbide (Ti3C2Tx MXene)]. United States. doi:10.1021/acs.chemmater.7b02847.
Alhabeb, Mohamed, Maleski, Kathleen, Anasori, Babak, Lelyukh, Pavel, Clark, Leah, Sin, Saleesha, and Gogotsi, Yury G. 2017. "Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene) [Guidelines for Synthesis and Processing of 2D Titanium Carbide (Ti3C2Tx MXene)]". United States. doi:10.1021/acs.chemmater.7b02847.
@article{osti_1399240,
title = {Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene) [Guidelines for Synthesis and Processing of 2D Titanium Carbide (Ti3C2Tx MXene)]},
author = {Alhabeb, Mohamed and Maleski, Kathleen and Anasori, Babak and Lelyukh, Pavel and Clark, Leah and Sin, Saleesha and Gogotsi, Yury G.},
abstractNote = {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. Furthermore we describe the experimental methods and best practices we use to synthesize the most studied MXene, titanium carbide (Ti3C2Tx), using different etchants and delamination methods. We also explain effects of synthesis parameters on the size and quality of Ti3C2Tx and suggest the optimal processes for the desired application.},
doi = {10.1021/acs.chemmater.7b02847},
journal = {Chemistry of Materials},
number = 18,
volume = 29,
place = {United States},
year = 2017,
month = 8
}

Journal Article:
Free Publicly Available Full Text
This content will become publicly available on August 25, 2018
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  • Two-dimensional transition metal carbides and nitrides (MXenes) are one of the largest and fastest growing families of materials. The presence of molecular hydrogen at ambient conditions in a MXene (Ti 3C 2T x, where T x represents a surface terminating species, including O, OH, and F) material is revealed here by inelastic and elastic neutron scatterings. The inelastic neutron-scattering spectrum measured at 5 K shows a peak at 14.6 meV, presenting a clear indication of the presence of parahydrogen in the MXene synthesized using 48% hydrofluoric acid and annealed at 110°C in vacuum prior to the measurement. An increase inmore » the measurement temperature gradually reduces the peak intensity and increases the peak width due to the mobility of the molecular hydrogen in confinement. The presence of molecular hydrogen is confirmed further from the observed elastic intensity drop in a fixed energy-window scan of elastic intensity measurements in the temperature range of 10–35 K. Using milder etching conditions, ion intercalation, or an increase in the annealing temperature all result in the absence of the trapped hydrogen molecules in MXene. Here, the results of this paper can guide the development of MXene materials with desired properties and improve our understanding of the behavior of MXenes in applications ranging from supercapacitors to hydrogen evolution reaction catalysis and hydrogen storage.« less
  • Here, noble metal (gold or silver) nanoparticles or patterned films are typically used as substrates for surface-enhanced Raman spectroscopy (SERS). Two-dimensional (2D) carbides and nitrides (MXenes) exhibit unique electronic and optical properties, including metallic conductivity and plasmon resonance in the visible or near-infrared range, making them promising candidates for a wide variety of applications. Herein, we show that 2D titanium carbide, Ti 3C 2T x, enhances Raman signal from organic dyes on a substrate and in solution. As a proof of concept, MXene SERS substrates were manufactured by spray-coating and used to detect several common dyes, with calculated enhancement factorsmore » reaching ~10 6. Titanium carbide MXene demonstrates SERS effect in aqueous colloidal solutions, suggesting the potential for biomedical or environmental applications, where MXene can selectively enhance positively charged molecules.« less
  • Silica-titania-phenolic resin hybrid fibers have been prepared from ethanol solutions of tetraethoxysilane (TEOS), titanium tetrakis(2,4-pentanedionate) (TTP), and novalac-type phenolic resins, where water and HCl have been added at a (TEOS + TTP):water:HCl molar ratio of 1:2:0.01, by sol-gel processing. The Si-to-Ti atomic ratio of the hybrid fibers was varied down to 10.4 by changing the amounts of TEOS and TTP in the starting solutions. Carbothermal reduction of both silica and titania components of the hybrid fibers has taken place at 1,500 C in an Ar flow, resulting in the formation of continuous {beta}-silicon carbide-titanium carbide hybrid fibers with Si-to-Ti atomicmore » ratios varied down to 9.9.« less