Delaminating Ti3C2 MXene by blossom of ZnIn2S4 microflowers for noble-metal-free photocatalytic hydrogen production

doi:10.1016/j.jmst.2021.12.028

Abstract

Abstract:

Herein, a novel strategy was exploited to achieve the delamination of Ti₃C₂ MXene multilayers into ultrathin flakes by blossom of ZnIn₂S₄ microflowers via a one-pot solvothermal method. There is no need to peel off the MXene bulk ahead of its combination with the semiconductor. The obtained ZnIn₂S₄/Ti₃C₂ binary composites were applied for visible-light-driven photocatalytic hydrogen production without noble metal cocatalyst, and the optimized sample exhibited a hydrogen-production efficiency of 978.7 μmol h ^{- 1} g ^{- 1} with the corresponding apparent quantum efficiency of 24.2% at 420 nm, which was 2.7 times higher than bare ZnIn₂S₄. Through the comprehensive analysis based on spectroscopy measurements, electrochemical techniques and energy band theory, such enhancement was mainly attributed to (1) the highly-exposed surface that was beneficial for the adequate exposure of reactive sites and (2) the intimate contact interface that favored the transfer of photogenerated carriers. This study provides a new way of thinking for synthesizing ultrathin MXene-based composite materials for noble-metal-free and highly-efficient photocatalysis applications.

Key words: ZnIn₂S₄, Ti₃C₂, Mxene, Photocatalysis, Hydrogen production

Weixin Huang, Zhipeng Li, Chao Wu, Hanjie Zhang, Jie Sun, Qin Li. Delaminating Ti₃C₂ MXene by blossom of ZnIn₂S₄ microflowers for noble-metal-free photocatalytic hydrogen production[J]. J. Mater. Sci. Technol., 2022, 120: 89-98.

Figures/Tables 11

Scheme 1. Schematic illustration of the preparation process of the ZnIn2S4/Ti3C2 composites.

Fig. 1. XRD patterns of (a) the Ti3AlC2, Ti3C2 and (b) the prepared ZnIn2S4 and ZTx samples. (c) Raman spectra of the ZnIn2S4, ZT10 and Ti3C2 samples.

Table 1. Actual Ti3C2 to ZnIn2S4 ratios in the composite and comparison of photocatalytic H2 production performance of the prepared samples.

Sample	Actual molar ratio of Ti₃C₂ to ZnIn₂S₄ (%)	Mass of sample for HER^a (mg)	A_BET (m² g ^{- 1})	R_H2 (μmol h ^{- 1})	R_H2 per mass (μmol h ^{- 1} g ^{- 1})	R_H2 per A_BET (μmol h ^{- 1} m ^{- 2})	AQE (%)
ZnIn₂S₄	0	100	58.4	36.4	364.4	6.2	9.5
ZT5	3.8	100	69.8	72.2	721.6	10.3	17.6
ZT10	6.6	100	73.2	97.9	978.7	13.4	24.2
ZT20	13.2	100	62.0	72.6	726.1	11.7	17.9
ZT40	24.5	100	61.1	58.5	585.4	9.6	12.3
ZT80	56.8	100	60.6	35.4	353.6	5.8	9.3

Fig. 2. (a) FESEM and (b) HRTEM images of the prepared ZT10 sample. (c) HAADF-STEM image of the ZT10 sample and the EDS mapping images of its Zn, In, S, and Ti atoms.

Fig. 3. FESEM images of the ZT10 sample with the solvothermal time for (a) 10 min, (b) 1 h, and (c) 12 h, respectively. (d) FESEM image of the ZT80 sample.

Fig. 4. (a) N2 adsorption/desorption isotherms and (b) the corresponding pore size distribution curves of the prepared ZnIn2S4 and ZTx samples.

Fig. 5. Photographs of (a) the automatic online trace gas analysis system (Labsolar-6A, Beijing Perfectlight Technology Co., Ltd.) and (b) the multi-channel photochemical reaction system (PCX-50B, Beijing Perfectlight Technology Co., Ltd.). (c) Dependence of the amount of H2 production on the concentration of the ZT10 sample in the system. (d) Comparison of the photocatalytic H2 production rates of the prepared samples.

Fig. 6. (a) Steady-state PL spectra of the ZnIn2S4, ZT5, ZT10, ZT40 and ZT80 samples and (inset) its local magnification. (b) Time-resolved transient photoluminescence decay of the ZnIn2S4 and ZT10 samples. (c) TPR plots and (d) EIS plots of the ZnIn2S4, ZT5, ZT10, ZT40 and ZT80 samples.

Fig. 7. High-resolution XPS spectra of (a) C 1 s, (b) Ti 2p, and (c) Zn 2p of the ZnIn2S4, ZT10 and Ti3C2 samples.

Fig. 8. (a) DRS spectra of the prepared samples and (b) corresponding Tauc plots of ZnIn2S4 and ZT10. Mott-Schottky plots of (c) ZnIn2S4 and (d) ZT10 at a frequency of 1000 Hz, 2000 Hz and 3000 Hz in Na2SO4 (0.5 M). (e) CPD values of the Ti3C2, ZT10, and ZnIn2S4 samples. (f) LSV curves of the ZnIn2S4 and ZT10 samples.

Fig. 9. Proposed photocatalytic H2 evolution mechanism over ZnIn2S4/Ti3C2 composite photocatalysts.

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Delaminating Ti₃C₂ MXene by blossom of ZnIn₂S₄ microflowers for noble-metal-free photocatalytic hydrogen production

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