MoS2/Zn3In2S6复合光催化剂构建: 高效提升可见光驱动甲酸制氢

doi:10.1016/S1872-2067(20)63584-7

催化学报 ›› 2021, Vol. 42 ›› Issue (1): 193-204.DOI: 10.1016/S1872-2067(20)63584-7

MoS₂/Zn₃In₂S₆复合光催化剂构建: 高效提升可见光驱动甲酸制氢

张素娟, 段世祥, 陈高礼, 孟苏刚, 郑秀珍, 樊佑, 付先亮, 陈士夫^*()

淮北师范大学清洁能源及绿色循环重点实验室, 安徽淮北235000

收稿日期:2020-02-23 接受日期:2020-04-13 出版日期:2021-01-18 发布日期:2021-01-18
通讯作者: 陈士夫
基金资助:
国家自然科学基金(51972134);国家自然科学基金(51472005);国家自然科学基金(51772118);安徽省杰出青年科学基金(1808085J24);安徽省高校优秀青年人才基金(gxyq2019029);安徽省高校自然科学研究项基金(KJ2019A0602);安徽省高校自然科学研究项基金(KJ2018A0387)

MoS₂/Zn₃In₂S₆composite photocatalysts for enhancement of visible light-driven hydrogen production from formic acid

Sujuan Zhang, Shixiang Duan, Gaoli Chen, Sugang Meng, Xiuzhen Zheng, You Fan, Xianliang Fu, Shifu Chen^*()

Key Laboratory of Clean Energy and Green Circulation, Huaibei Normal University, Huaibei 235000, Anhui, China

Received:2020-02-23 Accepted:2020-04-13 Online:2021-01-18 Published:2021-01-18
Contact: Shifu Chen
About author:^*Tel: +86-561-3802061; Fax: +86-561-3090518; E-mail: chshifu@chnu.edu.cn
Supported by:
National Natural Science Foundation of China(51972134);National Natural Science Foundation of China(51472005);National Natural Science Foundation of China(51772118);Natural Science Foundation of Anhui Province for Distinguished Young Scholars(1808085J24);Project of Anhui Province for Excellent Young Talents in Universities(gxyq2019029);Natural Science Foundation of Educational Committee of Anhui Province(KJ2019A0602);Natural Science Foundation of Educational Committee of Anhui Province(KJ2018A0387)

摘要/Abstract

摘要：

虽然传统的化石燃料依然能够满足当今快速工业化发展对能源的巨大需求, 但其固有的不可再生性及其燃烧产物对环境的污染, 严重阻碍了其在生产和生活中的广泛使用. 因此, 可持续清洁能源开发的研究已快速成为人类研究的热点. 氢是一种具备高热值、可持续等优点的清洁能源, 也兼备成本及污染低等优势. 甲酸(FA)以其无毒、低成本、氢含量高等优点, 是一种潜在的热门储氢材料, 而可见光占太阳光谱的43%左右. 因此, 开发高效可见光催化剂驱动FA制氢将是一种应对能源危机的有效途径.
许多传统光催化剂已被用于可见光催化FA制氢, 但制备成本高、过程复杂、条件苛刻及可见光响应差、稳定性和选择性差、有毒气体释放等缺点严重限制了其光催化性能. 光催化研究关键之一是实现光生电荷的高效率分离和转移, 从而光催化剂光催化性能的提高. Zn₃In₂S₆(ZIS6)因具有强可见光吸收、稳定性好及环保等特点正迅速成为光催化剂半导体的“明星”, 常与助催化剂(如贵金属Pt、Au、Pd等)复合形成异质结以促进光生载流子分离和提高其光催化活性, 但制备成本高等因素却严重限制其发展. 将成本低、化学稳定性好的MoS₂与其它半导体耦合也是提高半导体光催化剂性能的有效手段之一, 但高温、热处理时间长及有毒气体释放等却成了制约因素.
本文选用价格低廉的反应前驱体, 采用简单的一锅法水将MoS₂紧密地结合到ZIS6的表面, 热制备了一系列含有不同质量百分比MoS₂的MoS₂/Zn₃In₂S₆(MoS₂/ZIS6)复合光催化剂, 有效降低了制备成本和有毒气体(H₂S)的释放. 结果表明, 可见光照射下(λ > 400 nm), MoS₂的引入可大大提高ZIS6光生电荷分离效率及制氢活性, 尤其以0.5% MoS₂/ZIS6性能最优, 光催化制氢速率高达74.25 µmol·h^-1 (量子效率约2.9%), 约ZIS6的4.3倍(17.47 µmol·h ^-1). XRD结果表明, MoS₂/ZIS6样品中含有无定型MoS₂紧密固定在晶型ZIS6片状结构表面, 未影响ZIS6晶型, SEM表征也证实了此结果. 随后的TEM、HRTEM及EDX结果也进一步确认了各组成元素的存在和分布. 采用XPS对元素化学环境进行了分析, 通过S和Mo元素的成键能变化证实了MoS₂和ZIS6间的紧密接触. UV-Vis DRS测试表明, MoS₂/ZIS6可以利用可见光在适当带隙的基础上进行光催化制氢. 通过BET、PL和电化学技术研究了比表面积、光生电荷分离和传递速率等对光催化性能的影响. 最终, 结合上述表征结果成功阐述了可见光驱动FA制氢的反应机理.

关键词: 产氢, Zn₃In₂S₆, 甲酸, MoS₂, 光催化

Abstract:

Enhancing the separation efficiency of photogenerated carriers is propitious for the promotion of photocatalytic hydrogen production from formic acid decomposition. Herein, MoS₂/Zn₃In₂S₆ (MoS₂/ZIS6) composite photocatalysts containing varying mass percentages of MoS₂ were obtained by a straightforward synthetic method. The results confirmed that MoS₂, as a cocatalyst, markedly promoted the photogenerated charge separation efficiency and visible light-driven hydrogen production activity of ZIS6 (λ > 400 nm). Specifically, the as-prepared 0.5% MoS₂/ZIS6 photocatalyst exhibited the highest photocatalytic hydrogen production rate (74.25 µmol·h^-1), which was approximately 4.3 times higher than that of ZIS6 (17.47 µmol·h ^-1). The excellent performance of the 0.5% MoS₂/ZIS6 photocatalyst may be due to the fact that MoS₂ has a low Fermi energy level and can thus enrich photogenerated electrons from ZIS6, and furthermore reduce H⁺ derived from formic acid, to form hydrogen. The structure and morphology of the MoS₂/ZIS6 photocatalysts and the reactive species were determined by X-ray diffraction, transmission electron microscopy, and field emission scanning electron microscopy, among others; a plausible mechanistic rationale is discussed based on the results.

Key words: Hydrogen production, Zn₃In₂S₆, Formic acid, MoS₂, Photocatalysis

张素娟, 段世祥, 陈高礼, 孟苏刚, 郑秀珍, 樊佑, 付先亮, 陈士夫. MoS₂/Zn₃In₂S₆复合光催化剂构建: 高效提升可见光驱动甲酸制氢[J]. 催化学报, 2021, 42(1): 193-204.

Sujuan Zhang, Shixiang Duan, Gaoli Chen, Sugang Meng, Xiuzhen Zheng, You Fan, Xianliang Fu, Shifu Chen. MoS₂/Zn₃In₂S₆composite photocatalysts for enhancement of visible light-driven hydrogen production from formic acid[J]. Chinese Journal of Catalysis, 2021, 42(1): 193-204.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63584-7

https://www.cjcatal.com/CN/Y2021/V42/I1/193

图/表 15

	B1	T1/ns	B2	T2/ns	T/ns
1	4.389175	0.01489459	3.815503E-04	6.761111	0.2709953377
2	0.7557613	0.04515458	5.743187E-04	5.486072	0.5050377595

Fig. 1. XRD patterns of ZIS6, MoS2 and MoS2/ZIS6 samples and standard patterns of ZIS6 and MoS2.

Fig. 2. SEM (a, b), TEM (e), HRTEM (g), elemental mapping images and EDX analysis graph (j) of ZIS6; SEM (c, d), TEM (f), HRTEM (h, i), elemental mapping images and EDX analysis graph (k) of 0.5% MoS2/ZIS6.

Fig. 3. UV-Vis DRS spectra and photos (left inset) of ZIS6, 0.5% MoS2/ZIS6 and MoS2 photocatalysts and band gap energy (right inset) of ZIS6 and MoS2 samples.

Fig. 4. (a) Full XPS spectra of ZIS6, 0.5% MoS2/ZIS6 and MoS2; high resolution XPS spectra of Zn 2p (b), In 3d (c), S 2p (d), Mo 3d (e) in pure ZIS6, 0.5% MoS2/ZIS6 and MoS2.

Fig. 5. Steady-state (a), and time-resolved PL spectra (b) of ZIS6 and 0.5% MoS2/ZIS6.

Fig. 6. N2 adsorption-desorption isotherms and the pore size distribution of as-prepared ZIS6, MoS2 and 0.5% MoS2/ZIS6 samples.

Fig. 7. Comparison of H2 production rates of 0.1 g MoS2/ZIS6 composite photocatalysts containing different amounts of MoS2 from formic acid under visible light irradiation (λ > 400 nm).

Fig. 8. Photocatalytic H2 production activity of the 0.5% MoS2/ZIS6 sample under extended irradiation time.

Fig. 9. Comparison of quantum efficiencies based on hydrogen production amounts under a distinct wavelength illumination for 2 h with the 0.5% MoS2/ZIS6 photocatalyst.

Fig. 10. Comparison of transient photocurrent diagrams of pure ZIS6 and 0.5% MoS2/ZIS6 samples.

Fig. 11. Electrochemical impedance spectroscopy of ZIS6, MoS2 and 0.5% MoS2/ZIS6.

Fig. 12. Mott-Schottky plots of ZIS6 (a) and MoS2 (b) in 0.2 M Na2SO4.

Fig. 13. TPV (a) and TPC (b) spectra of ZIS6 and 0.5% MoS2/ZIS6 samples under a 355 nm laser pulse and power of 50 μJ/pulse. Insets show the schematic setup of TPV (a) and TPC (b) measurements, respectively.

Fig. 14. Possible charge transfer mechanism of hydrogen production from FA on the MoS2/ZIS6 photocatalyst.

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MoS₂/Zn₃In₂S₆复合光催化剂构建: 高效提升可见光驱动甲酸制氢

MoS₂/Zn₃In₂S₆composite photocatalysts for enhancement of visible light-driven hydrogen production from formic acid

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