多级结构形貌β-Bi2O3/BiOCOOH复合光催化剂的制备及其光催化性能

doi:10.11901/1005.3093.2019.471

材料研究学报

2020, Vol. 34

Issue (4): 311-320 DOI: 10.11901/1005.3093.2019.471

研究论文

本期目录 | 过刊浏览

多级结构形貌β-Bi₂O₃/BiOCOOH复合光催化剂的制备及其光催化性能

薛文兴¹, 谢丽燕²(

), 王万军³, 刘明华¹, 黄建辉²

1.福州大学环境与资源学院福州 350002
2.莆田学院环境与生物工程学院福建省新型污染物生态毒理效应与控制重点实验室;生态信息图谱福建省高校重点实验室莆田 351100
3.广东工业大学环境科学与工程学院环境卫生与污染控制研究所广州 510006

Preparation and Photocatalytic Properties of Composite Photocatalyst β-Bi2O3/BiOCOOH with Hierarchical Structure

XUE Wenxing¹, XIE Liyan²(

), WANG Wanjun³, LIU Minghua¹, HUANG Jianhui²

1.College of Environment and Resources, Fuzhou University, Fuzhou 350002, China
2.College of Environmental and Biological Engineering, Fujian Provincial Key Laboratory of Ecology-toxicological Effects & Control for Emerging Contaminants, Key Laboratory of Ecological Environment and Information Atlas, Fujian Provincial University, Putian University, Putian 351100, China
3.Institute of Environmental Health and Pollution Control, School of Environmental Science and Engineering, Guangdong University of Technology, Guangzhou 510006, China

引用本文:

薛文兴, 谢丽燕, 王万军, 刘明华, 黄建辉. 多级结构形貌β-Bi₂O₃/BiOCOOH复合光催化剂的制备及其光催化性能[J]. 材料研究学报, 2020, 34(4): 311-320.
Wenxing XUE, Liyan XIE, Wanjun WANG, Minghua LIU, Jianhui HUANG. Preparation and Photocatalytic Properties of Composite Photocatalyst β-Bi2O3/BiOCOOH with Hierarchical Structure[J]. Chinese Journal of Materials Research, 2020, 34(4): 311-320.

全文: PDF(10816 KB) HTML

摘要:

用水热法合成具有多级结构形貌的甲酸氧铋，将其作为自牺牲前驱体调节热处理温度制备出不同的产物，其中一种是具有可见光响应的新型β-Bi₂O₃/BiOCOOH复合光催化材料。使用X射线衍射(XRD)、紫外-可见漫反射光谱(UV-Vis DRS)、扫描电子显微镜(SEM)和光电化学响应等手段表征不同温度热处理后产物的晶型结构、光吸收性能、形貌、光电流等物理化学性质。以罗丹明B作为光催化活性评价的探针分子，研究了在不同温度热处理产物的可见光光催化性能。结果表明，热处理温度从250℃提高到330℃、400℃、450℃，甲酸氧铋发生以下转变：BiOCOOH→β-Bi₂O₃/BiOCOOH→β-Bi₂O₃→α-Bi₂O₃。在330℃和350℃热处理后的β-Bi₂O₃/BiOCOOH复合光催化剂可见光催化性能最优，其降解速率比β-Bi₂O₃、α-Bi₂O₃分别高6.7倍和100倍。对罗丹明B表现出最佳脱色率的样品，光照90 min的矿化率可达88%。与纯相物质(β-Bi₂O₃、BiOCOOH)相比β-Bi₂O₃/BiOCOOH复合材料具有更大的光电流响应和更小的阻抗。结合UV-vis DRS和莫特-肖特基曲线可推测，β-Bi₂O₃与BiOCOOH可紧密结合形成Z-型光催化结构，具有更高的光生载流子分离效率并实现光生电荷的分离。

关键词 ：复合材料, 可见光催化, 自牺牲前驱体, β-Bi₂O₃/BiOCOOH

Abstract：

The BiOCOOH with multi-layered structure was synthesized by hydrothermal method, and then was used as sacrificial precursor to prepare several different products through adjusting heat treatment temperatures, including a new type of composite photocatalytic material β-Bi₂O₃/BiOCOOH with visible light response. The crystal structure, optical absorption performance, morphology, photocurrent and other physical and chemical properties of the products were characterized by means of X-ray diffraction (XRD), UV-Vis DRS, scanning electron microscope (SEM), photoelectric chemical response and other characterization methods. Their photocatalytic activity was assessed via degradation test of Rhodamine B solution. The results show that when the heat treatment temperature gradually increased from 250℃ to 330℃, 400℃ and 450℃, the following transformation occurred: BiOCOOH→β-Bi₂O₃/BiOCOOH→β-Bi₂O₃→α-Bi₂O₃. The visible light catalytic performance of the composite photocatalyst β-Bi₂O₃/BiOCOOH is the best. The degradation rate of Rhodamine B in the presence of β-Bi₂O₃/BiOCOOH composite photocatalyst was 6.7 times and 100 times higher than those in the presence of β-Bi₂O₃and α-Bi₂O₃, respectively. The samples that showed the best decolorization rate for rhodamine B had a mineralization rate of 88% within 90 minutes of illumination. Electrochemical test results show that the composite β-Bi₂O₃/BiOCOOH has a larger photocurrent response and a smaller impedance than the plain materials β-Bi₂O₃ and BiOCOOH. In addition, by considering both of UV-Vis DRS and Mott-Shottky curves comprehensively, the positions of conduction and valence bands of β-Bi₂O₃ and BiOCOOH can be estimated respectively, and it is speculated that β-Bi₂O₃ and BiOCOOH can be closely combined to form z-type photocatalytic structure, thus having higher separation efficiency of photogenerated carriers and effective separation of photogenerated charges.

Key words： composite visible-light photocatalysis self-sacrificial precursor β-Bi₂O₃/BiOCOOH

收稿日期: 2019-10-13

ZTFLH:

O643.36

基金资助:福建省自然科学基金(No. 2019N0022);福建省自然科学基金(No. 2018J01439);莆田市科技局科技计划(No. 2016S1001);莆田市科技局科技计划(No. 2018NP2001);福建省教育厅科技项目(No. JT180468);福建省高校新世纪人才计划

作者简介: 薛文兴，男，1994年生，硕士生

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https://www.cjmr.org/CN/10.11901/1005.3093.2019.471 或 https://www.cjmr.org/CN/Y2020/V34/I4/311

图1 样品的制备流程图

图2 在不同温度热处理样品的XRD谱图

图3 不同样品的SEM照片

图4 β-Bi2O3/BiOCOOH样品的TEM和HRTEM照片

图5 不同样品的紫外可见分光光度图谱

图6 前驱体BiOCOOH、β-Bi2O3/BiOCOOH、β-Bi2O3和α-Bi2O3的N2吸-脱附等温线

图7 在330℃热处理样品β-Bi2O3/BiOCOOH降解RhB溶液、在400℃热处理样品β-Bi2O3降解RhB溶液、在不同温度热处理样品对RhB溶液的降解活性对比以及光催化降解反应的一级反应动力学拟合曲线

图8 β-Bi2O3/BiOCOOH光催化体系对罗丹明B溶液的TOC去除率

图9 BiOCOOH、β-Bi2O3和β-Bi2O3/BiOCOOH的光电流瞬态响应

图10 BiOCOOH、β-Bi2O3、α-Bi2O3和β-Bi2O3/BiOCOOH的Nyquist阻抗图

图11 BiOCOOH和β-Bi2O3的莫特-肖特基曲线

图12 β-Bi2O3/BiOCOOH复合材料在可见光下的电子-空穴分离示意图

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