Advances in nano research

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Calcium annealing approach to control of surface groups and formation of oxide in Ti3C2Tx MXene

  • Jung-Min Oh (R&D center, INNOMXENE Co.,Ltd.) ;
  • Su Bin Choi (Department of Smart Fab Technology, Sungkyunkwan University) ;
  • Taeheon Kim (School of Advanced Materials Engineering, Jeonbuk National University) ;
  • Jikwang Chae (R&D center, INNOMXENE Co.,Ltd.) ;
  • Hyeonsu Lim (Department of Strategy Planning, Jeonbuk Institute of Automotive Convergence Technology) ;
  • Jae-Won Lim (School of Advanced Materials Engineering, Jeonbuk National University) ;
  • In-Seok Seo (School of Advanced Materials Engineering, Jeonbuk National University) ;
  • Jong-Woong Kim (Department of Smart Fab Technology, Sungkyunkwan University)
  • Received : 2021.07.26
  • Accepted : 2023.03.07
  • Published : 2023.07.25
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Abstract

Ti3C2Tx MXene, a 2D material, is known to exhibit unique characteristics that are strongly dependent on surface termination groups. Here, we developed a novel annealing approach with Ca as a reducing agent to simultaneously remove F and O groups from the surface of multilayered MXene powder. Unlike H2 annealing that removes F effectively but has difficulty in removing O, annealing with Ca effectively removed both O and F. X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy revealed that the proposed approach effectively removed F and O from the MXene powder. The results of O/N analyses showed that the O concentration decreased by 57.5% (from 2.66 to 1.13 wt%). In addition, XPS fitting showed that the volume fraction of metal oxides (TiO2 and Al2O3) decreased, while surface termination groups (-O and -OH) were enhanced, which could increase the hydrophilic and adsorption properties of the MXene. These findings suggest that when F and O are removed from the MXene powder, the interlayer spacing of its lattice structure increases. The proposed treatment also resulted in an increase in the specific surface area (from 5.17 to 10.98 m2/g), with an increase in oxidation resistance temperature in air from ~436 to ~667 ℃. The benefits of this novel technology were verified by demonstrating the significantly improved cyclic charge-discharge characteristics of a lithium-ion battery with a Ca-treated MXene electrode.

Keywords

Acknowledgement

This work was supported by National Research Foundation of Korea (NRF) grants (Number 2020M3H4A3081895, 2022R1A2C1010353 and RS-2023-00247545) funded by the Korean government (MSIP). Further support was provided by the Industry Technology R&D program (20006511), funded By the Ministry of Trade, Industry & Energy (MOTIE, Korea).

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