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Advances in Nano Research
  Volume 15, Number 1, July 2023 , pages 1-13
DOI: https://doi.org/10.12989/anr.2023.15.1.001
 


Calcium annealing approach to control of surface groups and formation of oxide in Ti3C2Tx MXene
Jung-Min Oh, Su Bin Choi, Taeheon Kim, Jikwang Chae, Hyeonsu Lim, Jae-Won Lim, In-Seok Seo and Jong-Woong Kim

 
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 °C. 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.
 
Key Words
    deoxidation; lithium-ion battery; MXene; surface termination group; Ti3C2Tx
 
Address
Jung-Min Ohamd Jikwang Chae: R&D center, INNOMXENE Co.,Ltd., 66, Daehwa-ro 106beon-gil, Daedeok-gu, Daejeon 34365, Republic of Korea

Su Bin Choi: Department of Smart Fab Technology, Sungkyunkwan University, 2066 Seobu-ro, Jangan-gu, Suwon, Gyeonggi-do 16419, Republic of Korea

Taeheon Kim, Jae-Won Lim and In-Seok Seo : School of Advanced Materials Engineering, Jeonbuk National University, 567 Baekje-daero, Deokjin-gu, Jeonju 54896, Republic of Korea

Hyeonsu Lim: Department of Strategy Planning, Jeonbuk Institute of Automotive Convergence Technology, 6,
Dongjansan 2-gil, Gunsan 54158, Republic of Korea

Jong-Woong Kim: Department of Smart Fab Technology, Sungkyunkwan University, 2066 Seobu-ro, Jangan-gu, Suwon, Gyeonggi-do 16419, Republic of Korea/ School of Mechanical Engineering, Sungkyunkwan University, 2066 Seobu-ro, Jangan-gu, Suwon, Gyeonggi-do 16419, Republic of Korea

 

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