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Room-Temperature Carbide-Derived Carbon Synthesis by Electrochemical Etching of MAX Phases
Engineering Department, Drexel University, Philadelphia, USA.
Engineering Department, Drexel University, Philadelphia, USA.
Engineering Department, Drexel University, Philadelphia, USA.
Engineering Department, Drexel University, Philadelphia, USA.
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2014 (English)In: Angewandte Chemie International Edition, ISSN 1433-7851, E-ISSN 1521-3773, Vol. 126, no 19, 4977-4980 p.Article in journal (Refereed) Published
Abstract [en]

Porous carbons are widely used in energy storage and gas separation applications, but their synthesis always involves high temperatures. Herein we electrochemically selectively extract, at ambient temperature, the metal atoms from the ternary layered carbides, Ti3AlC2, Ti2AlC and Ti3SiC2 (MAX phases). The result is a predominantly amorphous carbide-derived carbon, with a narrow distribution of micropores. The latter is produced by placing the carbides in HF, HCl or NaCl solutions and applying anodic potentials. The pores that form when Ti3AlC2 is etched in dilute HF are around 0.5 nm in diameter. This approach forgoes energy-intensive thermal treatments and presents a novel method for developing carbons with finely tuned pores for a variety of applications, such as supercapacitor, battery electrodes or CO2 capture.

Place, publisher, year, edition, pages
John Wiley & Sons, 2014. Vol. 126, no 19, 4977-4980 p.
Keyword [en]
Carbide; Cyclovoltammetrie; Elektrochemie; Kohlenstoff; Oxidationen
National Category
Chemical Sciences Physical Chemistry
URN: urn:nbn:se:liu:diva-111125DOI: 10.1002/ange.201402513OAI: diva2:753513
Available from: 2014-10-08 Created: 2014-10-08 Last updated: 2014-10-17Bibliographically approved
In thesis
1. Synthesis and Characterization of 2D Nanocrystals and Thin Films of Transition Metal Carbides (MXenes)
Open this publication in new window or tab >>Synthesis and Characterization of 2D Nanocrystals and Thin Films of Transition Metal Carbides (MXenes)
2014 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Two dimensional (2D) materials have received growing interest because of their unique properties compared to their bulk counterparts. Graphene is the archetype 2D solid, but other materials beyond graphene, such as MoS2 and BN have become potential candidates for several applications. Recently, a new family of 2D materials of early transition metal carbides and carbonitrides (Ti2CTx, Ti3C2Tx, Ti3CNTx, Ta4C3Tx, and more), labelled MXenes, has been discovered, where T stands for the surface-terminating groups.

Before the present work, MXenes had only been synthesized in the form of exfoliated and delaminated powders, which is not suitable for electronic applications. In this thesis, I demonstrate the synthesis of MXenes as epitaxial thin films, a more suitable form for electronic and photonic applications. Results show that 2D epitaxial Ti3C2Tx films - produced by HF and NH4HF2 etching of magnetron sputter-grown Ti3AlC2 - exhibit metallic conductive behaviour down to 100 K and are 90% transparent to light in the visible-infrared range. The results from this work may open the door for MXenes as potential candidates for transparent conductive electrodes as well as in electronic, photonic and sensing applications.

MXenes have been shown to intercalate cations and molecules between their layers that in turn can alter the surface termination groups. There is therefore a need to study the surface chemistries of synthetized MXenes to be able to study the effect of intercalation as well as altering the surface termination groups on the electronic structure and chemical states of the elements present in MXene layers. X-ray Photoelectron Spectroscopy (XPS) in-depth characterization was used to investigate surface chemistries of Ti3C2Tx and Ti2CTx. This thesis includes the discussion of the effect of Ar+ sputtering and the number of layers on the surface chemistry of MXenes. This study serves as a baseline for chemical modification and tailoring of the surface chemistry groups to potential uses and applications.

New MXene phases, Nb2CTx and V2CTx, are shown in this thesis to be produced from HF chemical etching of Nb2AlC and V2AlC powders. Characterization of the produced MXenes was carried out using Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Transmission Electron Microscope (TEM) and XPS. Nb2CTx and V2CTx showed promising performance as electrodes for Li-ion batteries.

In this thesis, electrochemical etching was used in an attempt to produce 2D metal carbides (MXene) from their ternary metal carbides, Ti3SiC2, Ti3AlC2 and Ti2AlC MAX phases. MAX phases in the form of highly dense bulk produced by Hot Isostatic Press. Several etching solutions were used such as HF, NaCl and HCl. Unlike the HF chemical etching of MAX phases, which results in MXenes, the electrochemical etching resulted in Carbide Derived Carbon (CDC). Here, I show the characterization of the produced CDC using several techniques such as XRD, TEM, Raman spectroscopy, and XPS. Electrochemical characterization was performed in the form of cyclic voltammetry, which sheds light on the etching mechanism.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2014. 41 p.
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1679
National Category
Materials Chemistry Inorganic Chemistry
urn:nbn:se:liu:diva-111128 (URN)10.3384/lic.diva-111128 (DOI)978-91-7519-225-3 (print) (ISBN)
2014-10-24, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)

The series name Linköping Studies in Science and Technology Licentiate Thesis in this publication is incorrect. Correct name is Linköping Studies in Science and Technology. Thesis.

Available from: 2014-10-08 Created: 2014-10-08 Last updated: 2016-08-31Bibliographically approved

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