S型异质结BiOBr/ZnMoO4的构建及光催化降解性能研究

doi:10.15541/jim20220192

无机材料学报 ›› 2023, Vol. 38 ›› Issue (1): 62-70.DOI: 10.15541/jim20220192

S型异质结BiOBr/ZnMoO₄的构建及光催化降解性能研究

马心全(), 李喜宝(), 陈智, 冯志军, 黄军同

南昌航空大学材料科学与工程学院, 南昌 330063

收稿日期:2022-04-04 修回日期:2022-05-20 出版日期:2022-06-03 网络出版日期:2022-06-03
通讯作者: 李喜宝, 副教授. E-mail: lxbicf@126.com
作者简介:马心全(1997-), 男, 硕士研究生. E-mail: maxinquan_2022@163.com
基金资助:
国家自然科学基金(51962023);江西省自然科学基金(20212BAB204045)

BiOBr/ZnMoO₄ Step-scheme Heterojunction: Construction and Photocatalytic Degradation Properties

MA Xinquan(), LI Xibao(), CHEN Zhi, FENG Zhijun, HUANG Juntong

School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063, China

Received:2022-04-04 Revised:2022-05-20 Published:2022-06-03 Online:2022-06-03
Contact: LI Xibao, associate professor. E-mail: lxbicf@126.com
About author:MA Xinquan (1997-), male, Master candidate. E-mail: maxinquan_2022@163.com
Supported by:
National Natural Science Foundation of China(51962023);Natural Science Foundation of Jiangxi Province(20212BAB204045)

摘要/Abstract

摘要：

光催化被广泛用于去除水中的难降解有机污染物, 但是由于光生电子和空穴的复合率高, 抑制了半导体光催化剂的催化活性。本研究通过简便的溶剂热法成功制备了一种BiOBr/ZnMoO₄复合材料。通过结构分析、原位XPS、功函数测试、自由基捕获及电子顺磁共振(ESR)实验等证实了BiOBr/ZnMoO₄复合材料形成了S型异质结。实验结果表明, 适当ZnMoO₄含量的BiOBr/ZnMoO₄异质结可以显著提高BiOBr的光催化性能。与纯BiOBr、ZnMoO₄相比, 质量分数15% BiOBr/ZnMoO₄在可见光下表现出最佳的光催化活性, 双酚A的光催化降解率达到85.3% (90 min), 环丙沙星的光降解速率常数分别是BiOBr的2.6倍和ZnMoO₄的484倍。这可归因于BiOBr和ZnMoO₄之间形成了紧密的界面结合和S型异质结, 使得光生载流子可以实现有效的空间分离和转移。这项工作为定向合成Bi基S型异质结复合光催化材料提供了一种简便有效的方法, 对进一步理解Bi基多元异质结光催化材料的构效关系提供了新的理论和实验基础。

关键词: S型异质结, 内建电场, BiOBr, ZnMoO₄, 光催化

Abstract:

Photocatalysis is widely used for the removal of refractory organic pollutants in water, but the catalytic activity of semiconductor photocatalysts is significantly inhibited due to the high recombination rate of photogenerated electrons and holes. In this study, an S-scheme BiOBr/ZnMoO₄ composite was successfully prepared by a facile solvothermal method. The structure analysis, in-situ XPS, work function test, free radical capture and ESR experiment confirmed that the BiOBr/ZnMoO₄ composite formed an S-scheme heterojunction. The experimental results show that BiOBr/ZnMoO₄ heterojunction with appropriate ZnMoO₄ content can significantly improve the photocatalytic performance of BiOBr. Compared with pure BiOBr and ZnMoO₄, 15% BiOBr/ZnMoO₄ exhibits the best photocatalytic activity under visible light irradiation, and the photocatalytic degradation rate of bisphenol A reaches 85.3% (90 min). The rate constants of photodegradation of ciprofloxacin are 2.6 times that of BiOBr and 484 times that of ZnMoO₄, respectively. This can be attributed to the tight interfacial bonding between BiOBr and ZnMoO₄ and the formation of S-scheme heterojunction, which enables the efficient spatial separation and transfer of photogenerated carriers. This work provides a simple and efficient method for the directional synthesis of Bi-based S-scheme heterojunction photocatalytic materials, and provides a new theory and experimental basis for further understanding of the structure-activity relationship of Bi-based multi-heterojunction photocatalytic materials.

Key words: S-scheme heterojunction, internal electric field, BiOBr, ZnMoO₄, photocatalysis

中图分类号:

O643

马心全, 李喜宝, 陈智, 冯志军, 黄军同. S型异质结BiOBr/ZnMoO₄的构建及光催化降解性能研究[J]. 无机材料学报, 2023, 38(1): 62-70.

MA Xinquan, LI Xibao, CHEN Zhi, FENG Zhijun, HUANG Juntong. BiOBr/ZnMoO₄ Step-scheme Heterojunction: Construction and Photocatalytic Degradation Properties[J]. Journal of Inorganic Materials, 2023, 38(1): 62-70.

图/表 13

图1 BiOBr/ZnMoO4复合光催化剂的制备流程

Fig. 1 Preparation process of BiOBr/ZnMoO4 composite photocatalyst

图2 样品的XRD图谱(a)及2θ=29°~33°的局部放大图谱(b)

Fig. 2 XRD patterns of the samples (a) and corresponding partial enlarged pattern at 2θ=29°-33°(b)

图3 15% BiOBr/ZnMoO4样品的TEM照片(a, b)及其HRTEM照片(c); 元素分布分析(d~i)

Fig. 3 TEM images (a, b) and HRTEM images (c) and elemental mapping analyses (d-i) of 15% BiOBr/ZnMoO4 samples

图4 15% BiOBr/ZnMoO4的原位XPS谱图(a)及其Bi4f (b)、O1s (c)、Br3d (d)、Zn2p (e)和Mo3d (f)的高分辨率XPS图谱

Fig. 4 In-situ XPS spectra of 15% BiOBr/ZnMoO4 (a), and corresponding Bi4f (b), O1s (c), Br3d (d), Zn2p (e) and Mo3d (f) high-resolution XPS spectra

图5 可见光照射下不同催化剂对BPA的光降解(a)和相应的一阶动力学方程图(c); CIP的光降解(b)和相应的一阶动力学方程图(d); 15% BiOBr/ZnMoO4光降解BPA(e)和CIP(f)的紫外吸收光谱

Fig. 5 Photodegradation of BPA by different catalysts under visible light irradiation (a) and corresponding first-order kinetic equations (c); CIP photodegradation (b) and corresponding first-order kinetic equations (d); UV spectra of BPA(e) and CIP(f) photodegraded by 15% BiOBr/ZnMoO4

图6 BiOBr (a)、ZnMoO4 (b)和15% BiOBr/ZnMoO4(c)的功函数

Fig. 6 Work functions of BiOBr (a), ZnMoO4 (b) and 15% BiOBr/ZnMoO4(c)

图7 BiOBr和ZnMoO4接触前后IEF和带弯曲的形成以及光生电荷转移机制

Fig. 7 Formation of IEF, band bending and photogenerated charge transfer mechanism before and after BiOBr and ZnMoO4 contact

图8 15% BiOBr/ZnMoO4的自由基捕获实验

Fig. 8 Radical trapping experiment of 15% BiOBr/ZnMoO4

图9 BiOBr/ZnMoO4光催化剂的S型异质结光催化机理

Fig. 9 S-scheme heterojunction photocatalytic mechanism of BiOBr/ZnMoO4 photocatalyst

图S1 15% BiOBr/ZnMoO4降解BPA循环测试(a)和光催化循环前后的XRD谱(b)

Fig. S1 Cycling test (a) of 15% BiOBr/ZnMoO4 degradation of BPA and XRD spectra before and after photocatalytic cycling (b)

图S2 瞬态光电流响应曲线(a)和电化学阻抗谱(b)

Fig. S2 Transient photocurrent response curves (a) and electrochemical impedance spectra (b)

图S3 BiOBr (a)和ZnMoO4 (b)的Mott-Schottky曲线; 样品的UV-Vis DRS谱图(c); BiOBr和ZnMoO4的Tauc图(d)

Fig. S3 Mott-Schottky curves of BiOBr (a) and ZnMoO4 (b); UV-Vis DRS of samples (c); Tauc plots of BiOBr and ZnMoO4 (d)

图S4 15% BiOBr/ZnMoO4的ESR检测结果: DMPO-·OH (a)和DMPO-·O2- (b)

Fig. S4 ESR detection results of 15% BiOBr/ZnMoO4: DMPO-·OH (a) and DMPO-·O2- (b)

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S型异质结BiOBr/ZnMoO₄的构建及光催化降解性能研究

BiOBr/ZnMoO₄ Step-scheme Heterojunction: Construction and Photocatalytic Degradation Properties

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