二维介孔超薄Cd0.5Zn0.5S纳米片: 形成机制及光催化分解水制氢性能

doi:10.1016/S1872-2067(20)63593-8

催化学报 ›› 2021, Vol. 42 ›› Issue (1): 152-163.DOI: 10.1016/S1872-2067(20)63593-8

二维介孔超薄Cd_0.5Zn_0.5S纳米片: 形成机制及光催化分解水制氢性能

薛文华^a, 常文茜^a, 胡晓云^b, 樊君^a^,^#(), 刘恩周^a^,^*()

^a西北大学化工学院, 陕西西安710069
^b西北大学物理学院, 陕西西安710069

收稿日期:2020-02-17 接受日期:2020-03-31 出版日期:2021-01-18 发布日期:2021-01-18
通讯作者: 樊君,刘恩周
基金资助:
国家自然科学基金(21676213);国家自然科学基金(21476183);国家自然科学基金(11974276);国家自然科学基金(51372201);中国博士后科学基金(2016M600809);陕西省自然科学基础研究计划(2017JM2026);陕西省自然科学基础研究计划(2018JM5020)

2D mesoporous ultrathin Cd_0.5Zn_0.5S nanosheet: Fabrication mechanism and application potential for photocatalytic H₂ evolution

Wenhua Xue^a, Wenxi Chang^a, Xiaoyun Hu^b, Jun Fan^a^,^#(), Enzhou Liu^a^,^*()

^aSchool of Chemical Engineering, Northwest University, Xi’an 710069, Shaanxi, China
^bSchool of Physics, Northwest University, Xi’an 710069, Shaanxi, China

Received:2020-02-17 Accepted:2020-03-31 Online:2021-01-18 Published:2021-01-18
Contact: Jun Fan,Enzhou Liu
About author:^#E-mail: fanjun@nwu.edu.cn
^*Tel: +86-13759963944; E-mail: liuenzhou@nwu.edu.cn;
Supported by:
National Natural Science Foundation of China(21676213);National Natural Science Foundation of China(21476183);National Natural Science Foundation of China(11974276);National Natural Science Foundation of China(51372201);China Postdoctoral Science Foundation(2016M600809);Natural Science Basic Research Plan in Shaanxi Province of China(2017JM2026);Natural Science Basic Research Plan in Shaanxi Province of China(2018JM5020)

摘要/Abstract

摘要：

太阳光驱动的光催化分解水产氢是一种绿色制氢技术, 并以氢为载体可实现太阳能向化学能的转化. 目前开发高效、稳定的可见光催化剂仍是本领域的研究热点. 在各类光催化材料中, Cd_0.5Zn_0.5S固溶体比TiO₂及g-C₃N₄具有更优异的光催化产氢活性, 但它一般为团聚了的纳米颗粒或纳米微球, 表面积小, 比表面反应迟缓, 从而限制了其实际应用. 通常, 超薄多孔二维结构光催化剂具有高比表面积, 能够为反应物分子与催化剂之间提供大量接触界面并促进传质, 此外, 特定晶面暴露赋予了其大量不饱和配位表面原子, 使反应物分子更容易在催化剂表面吸附活化, 提升表面催化反应动力学. 本文首先采用乙二胺与水的混合溶液制备了无机有机杂化的硫化锌-乙二胺(记为:ZnS(en)_0.5). 随后, 分别以ZnS(en)_0.5为硬模板、以乙二醇为反应介质、氯化镉为镉源, 通过溶剂热阳离子交换得到了无机有机杂化的Cd_0.5Zn_0.5S(en)_x中间产物. 最后, 将Cd_0.5Zn_0.5S(en)_x在纯水中进行水热反应脱除晶格内乙二胺分子得到了2D介孔超薄Cd_0.5Zn_0.5S纳米片. TEM测试发现, 纳米片表面存在大量孔洞, 其主要源于Cd_0.5Zn_0.5S(en)_x的相变过程及其晶格内乙二胺分子的逃逸导致的晶格畸变. AFM观察结果表明, 最终产物Cd_0.5Zn_0.5S纳米片厚度约为1.5 nm; 其比表面积可达63.5 m²/g, 几乎是相应纳米颗粒的两倍. 以三乙醇胺(TEOA)为牺牲剂时, Cd_0.5Zn_0.5S纳米片的产氢速率达到19.1 mmol·h^-1·g^-1, 是相应纳米颗粒的两倍多. 即使在纯水中, Cd_0.5Zn_0.5S纳米片产氢速率仍可达到1395 μmol·h^-1·g^-1, 超过了目前所报道的未加修饰的光催化剂的活性. 其优异的活性源于其独特的结构优势, 包括载流子迁移距离的缩短、表面不饱合原子及比表面积的增大. 但在纯水中其严重的光腐蚀仍然亟待克服. 此外, 为进一步增强其活性, 通过机械复合的方法得到了NiCo₂S₄/Cd_0.5Zn_0.5S二元复合光催化剂, 其在TEOA为牺牲剂时制氢速率可达62.2 mmol·h^-1·g^-1, 在纯水制氢速率达到2436 μmol·h ^-1·g^-1. 电化学、UPS及EPR分析表明, NiCo₂S₄与Cd_0.5Zn_0.5S纳米片间形成了肖特基接触, 进一步促进了载流子分离能力, 提高了复合物的产氢活性. 以本工作为基础, 还可制备其他高活性的CdZnS-基功能光催化材料用于太阳能转化或其他领域.

关键词: 介孔, 超薄, Cd_0.5Zn_0.5S纳米片, 光催化, 产氢

Abstract:

Two-dimensional mesoporous ultrathin Cd_0.5Zn_0.5S nanosheets with a thickness of ~1.5 nm were fabricated using a multistep chemical transformation strategy involving inorganic-organic hybrid ZnS-ethylenediamine (denoted as ZnS(en)_0.5) as a hard template. Inorganic-organic hybrid ZnS(en)_0.5, Cd_0.5Zn_0.5S(en)_x, and Cd_0.5Zn_0.5S nanosheets were sequentially fabricated, and their transformation processes were analyzed in detail. The fabricated Cd_0.5Zn_0.5S nanosheets exhibited high photocatalytic hydrogen evolution reaction activity in the presence of a sacrificial agent. The Cd_0.5Zn_0.5S nanosheets exhibited remarkably high H₂ production activity of ~1395 μmol∙h^-1∙g^-1 in pure water with no co-catalyst, which is the highest value reported thus far for bare photocatalysts, to the best of our knowledge. The high activity of these nanosheets is attributed to their distinct nanostructure (e.g., short transfer distance of photoinduced charge carriers, large number of unsaturated surface atoms, and large surface area). Moreover, ternary NiCo₂S₄ nanoparticles were employed to facilitate the charge separation and enhance the surface kinetics of H₂ evolution. The H₂ production rate reached ~62.2 and ~2436 μmol∙h^-1∙g^-1 in triethanolamine and pure water, respectively, over the NiCo₂S₄/Cd_0.5Zn_0.5S heterojunctions. The result indicated that the Schottky junction was critical to the enhanced activity. The proposed method can be used for fabricating other highly efficient CdZnS-based photocatalysts for solar-energy conversion or other applications.

Key words: Mesoporous, Ultrathin, Cd_0.5Zn_0.5S nanosheets, Photocatalysis, Hydrogen evolution

薛文华, 常文茜, 胡晓云, 樊君, 刘恩周. 二维介孔超薄Cd_0.5Zn_0.5S纳米片: 形成机制及光催化分解水制氢性能[J]. 催化学报, 2021, 42(1): 152-163.

Wenhua Xue, Wenxi Chang, Xiaoyun Hu, Jun Fan, Enzhou Liu. 2D mesoporous ultrathin Cd_0.5Zn_0.5S nanosheet: Fabrication mechanism and application potential for photocatalytic H₂ evolution[J]. Chinese Journal of Catalysis, 2021, 42(1): 152-163.

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https://www.cjcatal.com/CN/Y2021/V42/I1/152

图/表 12

Fig. 1. Preparation of the Cd0.5Zn0.5S nanosheets.

Fig. 2. (a) X-ray diffraction (XRD) patterns of ZnS(en)0.5 prepared with different Zn salts, (b) XRD patterns of ZnS(en)0.5, Cd0.5Zn0.5S(en)x and Cd0.5Zn0.5S nanosheets.

Fig. 3. FT-IR spectra of Cd0.5Zn0.5S nanosheets, Cd0.5Zn0.5S(en)x, ZnS(en)0.5, and dissociative en molecules.

Fig. 4. TEM images of ZnS(en)0.5 prepared with Zn(NO3)2 (a-c), Cd0.5Zn0.5S(en)x (d-f), and Cd0.5Zn0.5S (g-i) nanosheets; (j) EDS line scanning pattern and the corresponding elemental composition of the Cd0.5Zn0.5S nanosheets; (k) Atomic force microscopy (AFM) image of the prepared Cd0.5Zn0.5S nanosheets.

Fig. 5. High-resolution XPS spectra of Cd0.5Zn0.5S nanosheets and Cd0.5Zn0.5S(en)x.

Fig. 6. N2 adsorption-desorption isotherms and pore-size distributions.

Fig. 7. UV-vis absorption spectra of the prepared samples.

Fig. 8. (a) Photocatalytic performance of the Cd0.5Zn0.5S nanoparticles and Cd0.5Zn0.5S(en)x and Cd0.5Zn0.5S nanosheets. (b) H2 production over various NiCo2S4/Cd0.5Zn0.5S heterojunctions. (c, d) Wavelength-dependent photocatalytic H2 production over 7%-NiCo2S4/Cd0.5Zn0.5S. (e) H2 production over the samples under visible-light irradiation. (f) H2 production in pure water over Cd0.5Zn0.5S nanoparticles, Cd0.5Zn0.5S nanosheets, and 7%-NiCo2S4/Cd0.5Zn0.5S.

Table 1 N2 adsorption-desorption results.

Samples	Specific surface area (m²/g)	Pore diameter (nm)
Cd_0.5Zn_0.5S particles	35.1	4.6
Cd_0.5Zn_0.5S nanosheets	62.4	20.6
Cd_0.5Zn_0.5S(en)_x	121.6	7.2
7%-NiCo₂S₄/Cd_0.5Zn_0.5S	65.9	19.8

Fig. 9. Photocurrent density-time curves (a), Nyquist plots (b), HER polarization curves (c), and Tafel plots (d) for the two samples.

Fig. 10. (a) X-ray photoelectron valence-band (VB) spectra of the Cd0.5Zn0.5S nanosheets. (b) UV photoelectron spectrum of the Cd0.5Zn0.5S nanosheets. (c) UV photoelectron spectrum of the NiCo2S4 nanoparticles.

Fig. 11. PL spectra after ?OH detection (a, b) and in situ EPR spectra (c, d) of the samples, (e, f) PL spectra of the samples and the charge-transfer route of the binary composites.

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二维介孔超薄Cd_0.5Zn_0.5S纳米片: 形成机制及光催化分解水制氢性能

2D mesoporous ultrathin Cd_0.5Zn_0.5S nanosheet: Fabrication mechanism and application potential for photocatalytic H₂ evolution

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二维介孔超薄Cd0.5Zn0.5S纳米片: 形成机制及光催化分解水制氢性能

2D mesoporous ultrathin Cd0.5Zn0.5S nanosheet: Fabrication mechanism and application potential for photocatalytic H2 evolution

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二维介孔超薄Cd_0.5Zn_0.5S纳米片: 形成机制及光催化分解水制氢性能

2D mesoporous ultrathin Cd_0.5Zn_0.5S nanosheet: Fabrication mechanism and application potential for photocatalytic H₂ evolution