Effects of Preparation Conditions on the Morphologies, Structures and Electrochemical Properties of MXene†

doi:10.7503/cjcu20180783

Abstract

Abstract:

Using Ti₃AlC₂ as precursor, multilayered Ti₃C₂T_x were prepared and intercalated in one process with LiF+HCl as etchant, and then single or few layers of two-dimensional(2D) MXene flakes were delaminated with following sonication. The studies were focused on the effects of etching and delamination conditions by tuning the ratios of etchant/Ti₃AlC₂(molar ratio) and the sonication time on the morphologies, structures and electrochemical properties of two dimensional crystal flakes of Ti₃C₂T_x. The results showed that selecting appropriate fabrication conditions is crucial to the structures and properties of MXene flakes. It is shown that the MXene obtained with 6 mol/L HCl, the LiF/Ti₃AlC₂ molar ratio of 7.5 and the sonication time of 1 h which named FMX7.5-6' displayed a small lattice constant and a large flake size up to 1 μm. It also had a high content of oxygen-containing functional groups and demonstrated the best electrochemical properties. At the current density of 0.5 A/g, it demonstrated a high specific capacity of 342 F/g and its capacity could reach 244 F/g at the current density of 20 A/g. The specific capacity could remain 87% of the original value after 10000 cycling test at the current density of 1 A/g, showing a good rate and stability performance.

Key words: MXene, Ti₃C₂T_x, Etching, Exfoliation, Electrochemical property

CLC Number:

O646

TrendMD:

CHEN Yaoyan,ZHAO Xin,WANG Zhe,DONG Jie,ZHANG Qinghua. Effects of Preparation Conditions on the Morphologies, Structures and Electrochemical Properties of MXene^†[J]. Chem. J. Chinese Universities, 2019, 40(6): 1249.

Figures/Tables 12

Scheme 1 Schematic of preparation process of MXene flakes by etching and delamination

Fig.1 SEM images of Ti3AlC2 powder(A), MMX7.5-6(B), MMX7.5-9(C) and MMX12-6(D) The insets in (B—D) show the multilayered powder in water after handshaking and washing to pH≥6(i) and the dried multilayered powder of Ti3C2Tx(ii).

Fig.2 TEM images of FMX7.5-6(A), FMX7.5-9(B), FMX12-6(C), FMX7.5-6'(D), FMX7.5-9'(E) and FMX12-6'(F)

Fig.3 Particle size distribution of Ti3C2Tx with sonication for the first times(A) and the second times(B) and concentration distribution of colloidal aqueous solutions of Ti3C2Tx obtained after sonicating for the first times(left) and the second times(right)(C)

Fig.4 SEM images of fracture surfaces of the dried films (A) FMX7.5-6; (B) FMX7.5-9; (C) FMX12-6; (D) FMX7.5-6'; (E) FMX7.5-9'; (F) FMX12-6'.

Fig.5 XRD patterns of multilayered MXene powder(A) and the dried films(B)

Fig.6 XPS surveys of FMX7.5-6’(a), FMX7.5-9’(b) and FMX12-6’(c)

Fig.7 C1s(A) and O1s(B) XPS spectra of FMX7.5-6’(a), FMX7.5-9’(b), FMX12-6’(c) and Ti2p(C) and F1s(D) XPS spectra of FMX7.5-6’

Fig.8 CV curves of all the MXene films at a scan rate of 10 mV/s(A) and FMX7.5-6’ at different scan rates(B)

Fig.9 Galvanostatic charge-discharge curves of all the films at a current density of 0.5 A/g(A) and FMX7.5-6' at different current densities(B)

Fig.10 Gravimetric rate performances(A) and Nyquist plots(B) of all the MXene films

Fig.11 Capacitance retention rate of FMX7.5-6' at a current density of 1 A/g

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