有机胺表面修饰的一维CdSe0.8S0.2-DETA/二维SnNb2O6 S型异质结及其可见光光催化CO2还原性能

doi:10.1016/S1872-2067(20)63784-6

催化学报 ›› 2022, Vol. 43 ›› Issue (2): 255-264.DOI: 10.1016/S1872-2067(20)63784-6

有机胺表面修饰的一维CdSe_0.8S_0.2-DETA/二维SnNb₂O₆ S型异质结及其可见光光催化CO₂还原性能

杨辉, 张金锋^#(), 代凯^*()

淮北师范学院物理与电子信息学院, 绿色和精准合成化学及应用教育部重点实验室, 安徽淮北 235000

收稿日期:2021-01-20 接受日期:2021-01-20 出版日期:2022-02-18 发布日期:2021-02-22
通讯作者: 张金锋,代凯
基金资助:
国家自然科学基金(51572103);国家自然科学基金(51973078);安徽省杰出青年基金(1808085J14);安徽省教育厅重大项目(KJ2020ZD005);安徽省省级教学团队(2019jxtd062);安徽省教育厅重点项目(KJ2019A0595)

Organic amine surface modified one-dimensional CdSe_0.8S_0.2-diethylenetriamine/two-dimensional SnNb₂O₆ S-scheme heterojunction with promoted visible-light-driven photocatalytic CO₂ reduction

Hui Yang, Jin feng Zhang^#(), Kai Dai^*()

Key Laboratory of Green and Precise Synthetic Chemistry and Applications, Ministry of Education, School of Physics and Electronic Information, Huaibei Normal University, Huaibei 235000, Anhui, China

Received:2021-01-20 Accepted:2021-01-20 Online:2022-02-18 Published:2021-02-22
Contact: Jin feng Zhang, Kai Dai
Supported by:
This work was supported by the National Natural Science Foundation of China(51572103);This work was supported by the National Natural Science Foundation of China(51973078);the Distinguished Young Scholar of Anhui Province(1808085J14);the Major projects of Education Department of Anhui Province(KJ2020ZD005);Anhui Provincial Teaching Team(2019jxtd062);the Key Foundation of Educational Commission of Anhui Province(KJ2019A0595)

摘要/Abstract

摘要：

近年来, 随着人口的增加, 汽车尾气的排放和化石燃料的燃烧加剧, 大气中的二氧化碳含量持续增加. 光催化技术是根本上解决上述问题的有效方法之一. 但目前光催化技术存在催化效率低、载流子易复合等缺点. 二维SnNb₂O₆纳米片能够有效缩短光生电子从材料内部到材料表面的传输距离, 减少电子和空穴在光催化剂中的复合. 但SnNb₂O₆的带隙较宽, 导致可见光吸收率较低, 而且在单一的半导体材料中, 强氧化还原能力和高可见光吸收能力难以共存. CdSe_xS_1-_x-DETA是一种直接带隙半导体, 在可见光范围内可调节带隙. 为了提高SnNb₂O₆的光催化活性和光吸收范围, 在两种半导体材料之间设计异质结是一种有效的方法. 其中, 梯型(S型)异质结可以有效促进光生电子-空穴对的分离和转移, 并保持强大的氧化和还原能力, 在有效降低电子空穴对的复合速率的同时, 增强光催化剂的活性和稳定性.
本文通过溶剂热法设计制备了S型CdSe_0.8S_0.2-DETA/SnNb₂O₆异质结构材料, 利用X射线衍射(XRD)可以观察到除CdSe_0.8S_0.2-DETA和SnNb₂O₆物相外, 没有其它组分. 采用扫描电子显微镜和透射电子显微镜(TEM)进一步观察了光催化剂的结构和形貌, 结果表明, 一维的CdSe_0.8S_0.2-DETA生长在二维SnNb₂O₆纳米片上; 能谱分析也证实该催化剂仅包含CdSe_0.8S_0.2-DETA和SnNb₂O₆中的元素, 无其它杂质; TEM的晶格条纹进一步表明两种物质是复合在一起的, 不是机械的混合物. 紫外可见光漫反射光谱(UV-Vis)结果表明, CdSe_0.8S_0.2-DETA和SnNb₂O₆的吸收带边分别为1.71和2.52 eV. 随着复合样品中CdSe_0.8S_0.2-DETA含量的增加, 其可见光吸收范围增大. 光电流和阻抗响应图谱表明, CdSe_0.8S_0.2-DETA/SnNb₂O₆复合材料具有较高的光响应和较低的阻抗, 有利于电子空穴的运输. 光催化CO₂还原测试结果表明, 30%CdSe_0.8S_0.2-DETA/SnNb₂O₆催化CO₂还原生成CO的产率(17.31 μmol·g ^-1·h ^-1)最高, 分别是SnNb₂O₆ (6.2 μmol·g ^-1·h ^-1)和CdSe_0.8S_0.2-DETA (3.6 μmol·g ^-1·h ^-1)的2.8倍和4.8倍. XRD测试结果表明, 反应后光催化剂的与新鲜光催化剂的衍射峰基本相符. 催化剂经过4次循环测试后催化性能基本稳定, 说明光催化剂具有较好的稳定性. XPS表征结果显示, 相对于纯的CdSe_0.8S_0.2-DETA与SnNb₂O₆,复合材料中Cd, Se与S的结合能降低, 周围的电子密度增大, 而复合材料中Sn, Nb与O的结合能增加, 周围的电子密度降低, 这表明电子从SnNb₂O₆到CdSe_0.8S_0.2-DETA的转移路径遵循S型异质结机理. 综上, 本文提供了一种简单的制备S型光催化方法, 可以优化能带结构以促进光生载流子的分离, 从而实现高效率的二氧化碳还原.

关键词: 光催化, CdSe_xS_1-_x-DETA, SnNb₂O₆, 梯型, CO₂还原

Abstract:

Achieving a strong redox ability and high visible-light absorption ability in a single semiconductor material is difficult. Designing a heterojunction between two semiconductor materials is a feasible method. The new step (S-scheme) heterojunction can effectively promote the separation and transfer of photogenerated electron-hole pairs and retain strong redox ability. We designed and prepared a CdSe_0.8S_0.2-diethylenetriamine (DETA)/SnNb₂O₆ heterostructure material via the solvothermal method. When CdSe_0.8S_0.2-DETA and SnNb₂O₆ form an S-scheme heterojunction, 30%CdSe_0.8S_0.2-DETA/SnNb₂O₆ exhibits the highest CO production rate (17.31 μmol·g ^-1·h ^-1), which is factors of 2.8 and 4.8 higher than that of traditional solvothermal SnNb₂O₆(6.2 μmol·g ^-1·h ^-1) and CdSe_0.8S_0.2-DETA (3.6 μmol·g ^-1·h ^-1), respectively. X-ray photoelectron spectroscopy characterization data provided evidence that the transfer pathway of space charge in the CO₂ reduction process was in accordance with the S-scheme. This research provides a simple strategy through which one can optimize the band structure to promote the separation of photogenerated carriers and achieve a high efficiency of CO₂ reduction.

Key words: Photocatalysis, CdSe_xS_1-x-DETA, SnNb₂O₆, Step-scheme, CO₂ reduction

杨辉, 张金锋, 代凯. 有机胺表面修饰的一维CdSe_0.8S_0.2-DETA/二维SnNb₂O₆ S型异质结及其可见光光催化CO₂还原性能[J]. 催化学报, 2022, 43(2): 255-264.

Hui Yang, Jin feng Zhang, Kai Dai. Organic amine surface modified one-dimensional CdSe_0.8S_0.2-diethylenetriamine/two-dimensional SnNb₂O₆ S-scheme heterojunction with promoted visible-light-driven photocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2022, 43(2): 255-264.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63784-6

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图/表 8

Fig. 1. Schematic of the synthesis of CdSe0.8S0.2-DETA/SnNb2O6 nanocomposite.

Fig. 2. XRD patterns of SnNb2O6 and CdSe0.8S0.2-DETA/SnNb2O6 photocatalysts.

Fig. 3. (a-c) Field emission scanning electron microscopy images of SnNb2O6, CdSe0.8S0.2-DETA, and 30%CdSe0.8S0.2-DETA/SnNb2O6; (d,e) HRTEM images of 30%CdSe0.8S0.2-DETA/SnNb2O6. (f-n) EDS elemental mapping of 30%CdSe0.8S0.2-DETA/SnNb2O6.

Fig. 4. XPS spectra of pure CdSe0.8S0.2-DETA, SnNb2O6, and 30%CdSe0.8S0.2-DETA/SnNb2O6 nanocomposite: (a) Survey spectrum; (b) O 1s; (c) Nb 3d; (d) Sn 3d; (e) Se 3d; (f) S 2p; (g) Cd 3d and N 1s.

Fig. 5. (a) UV-visible diffuse reflectance spectra of different photocatalysts. (b) Plots of (αhν)2 vs. photon energies (hν) for CdSe0.8S0.2-DETA and plots of (αhν)1/2 vs. photon energies (hν) for SnNb2O6. (c,d) Valence-band spectra of CdSe0.8S0.2-DETA and SnNb2O6.

Fig. 6. Transient photocurrent responses (a) and Nyquist plot of electrochemical impedance spectra (b) of SnNb2O6, CdSe0.8S0.2-DETA and 30%CdSe0.8S0.2-DETA/SnNb2O6 nanocomposite.

Fig. 7. (a) Photocatalytic CO2 reduction activities of different samples. (b) Stability tests of CdSe0.8S0.2-DETA, SnNb2O6, and 30%CdSe0.8S0.2-DETA/SnNb2O6 for four consecutive cycles. (c) CO2 photoreduction performance of the system under varied conditions. (d) XRD patterns of 30%CdSe0.8S0.2-DETA/SnNb2O6 before and after testing.

Fig. 8. Schematic of the charge transfer pathway of 30%CdSe0.8S0.2-DETA/SnNb2O6.

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有机胺表面修饰的一维CdSe_0.8S_0.2-DETA/二维SnNb₂O₆ S型异质结及其可见光光催化CO₂还原性能

Organic amine surface modified one-dimensional CdSe_0.8S_0.2-diethylenetriamine/two-dimensional SnNb₂O₆ S-scheme heterojunction with promoted visible-light-driven photocatalytic CO₂ reduction

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