鸟巢状Bi/β-Bi2O3 异质结的制备及其可见光催化性能

doi:10.11901/1005.3093.2023.430

材料研究学报

2024, Vol. 38

Issue (7): 549-560 DOI: 10.11901/1005.3093.2023.430

研究论文

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鸟巢状Bi/β-Bi₂O₃ 异质结的制备及其可见光催化性能

周慧¹, 杜彬¹, 杨鹏斌¹, 金党琴¹, 肖伽励¹, 沈明²(

), 王升文¹

^1.扬州工业职业技术学院化学工程学院扬州 225127
^2.扬州大学化学化工学院扬州 225002

Sodium Gluconate Assisted Synthesis of Nest-like Bi/β-Bi₂O₃ Heterojunction and Its Visible-light Driven Photocatalytic Activities

ZHOU Hui¹, DU Bin¹, YANG Pengbin¹, JIN Dangqin¹, XIAO Jiali¹, SHEN Ming²(

), WANG Shengwen¹

^1.School of Chemical Engineering, Yangzhou Polytechnic Institute, Yangzhou 225127, China
^2.College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002, China

引用本文:

周慧, 杜彬, 杨鹏斌, 金党琴, 肖伽励, 沈明, 王升文. 鸟巢状Bi/β-Bi₂O₃ 异质结的制备及其可见光催化性能[J]. 材料研究学报, 2024, 38(7): 549-560.
Hui ZHOU, Bin DU, Pengbin YANG, Dangqin JIN, Jiali XIAO, Ming SHEN, Shengwen WANG. Sodium Gluconate Assisted Synthesis of Nest-like Bi/β-Bi₂O₃ Heterojunction and Its Visible-light Driven Photocatalytic Activities[J]. Chinese Journal of Materials Research, 2024, 38(7): 549-560.

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摘要:

在葡萄糖酸钠的辅助下用水热法制备鸟巢状含铋前驱体，研究了水热温度和反应物的浓度对其形貌和组成的影响及其生成机理。在150~400℃将前驱体煅烧制备出Bi/β-Bi₂O₃异质结分等级微纳结构。将前驱体煅烧使其分解生成Bi₂O₃，葡萄糖酸生成的碳将Bi³⁺原位还原为单质Bi。煅烧过程中的相变为：前驱体→Bi/β-Bi₂O₃(150~280℃)→Bi/β-Bi₂O₃/α-Bi₂O₃(300~350℃)→Bi(400℃)。以盐酸左氧氟沙星(LVFH)的降解为探针反应，研究了样品的可见光催化性能。结果表明：在280℃将前驱体煅烧制备的鸟巢状Bi/β-Bi₂O₃异质结材料具有最好的可见光催化活性，用可见光照射140 min对LVFH降解率达到97.75%。其具有较优异的光催化性能，可归因于鸟巢状分等级结构和原位生成的Bi纳米粒子的SPR效应提高了可见光的吸收并促进了光生载流子的分离。这种Bi/β-Bi₂O₃异质结光催化剂，还具有良好的可循环使用性能。

关键词 ：复合材料, Bi/β-Bi₂O₃, 可见光催化, 葡萄糖酸钠, 异质结, 盐酸左氧氟沙星

Abstract：

The nest-like bismuth-containing precursor was prepared by hydrothermal method with sodium gluconate as auxiliaries. The effect of the hydrothermal temperature and reactant concentration on the morphology and composition of the prepared precursor were systematically studied, and the formation mechanism of the precursor was elucidated. Then, calcination of the precursor was carried out at 150^oC~400^oC, during which the precursor decomposed to Bi₂O₃. At the same time, the carbon generated by high-temperature carbonization of the gluconic acid involved in the skeleton of the precursor can in situ reduce Bi³⁺ to Bi nanoparticles. The phase transition during calcination process can be described as: precursor→Bi/β-Bi₂O₃ (150^oC~280^oC) →Bi/β-Bi₂O₃/α-Bi₂O₃ (300^oC~350^oC)→Bi (400^oC). The degradation of levofloxacin hydrochloride (LVFH) was used as a probe to evaluate the visible-light photocatalytic performance of the as-prepared Bi/β-Bi₂O₃ heterojunctions. Among others, the Bi/β-Bi₂O₃ heterojunction obtained at 280^oC exhibited the best visible-light photocatalytic activity, and the degradation rate of LVFH can reach 97.75% after 140 min of visible-light irradiation. Its superior photocatalytic performance was attributed to the nest-like hierarchical structure and the SPR effect of the in situ generated Bi-nanoparticles, which improved visible-light harvesting and promoted the separation of photogenerated carriers. In addition, the Bi/β-Bi₂O₃ heterojunction photocatalyst showed good recyclable and reusable performance.

Key words： composite Bi/β-Bi₂O₃ visible-light photocatalysis sodium gluconate heterojunction levofloxacin hydrochloride

收稿日期: 2023-08-29

ZTFLH:

O643.36

基金资助:国家自然科学基金(21673201);江苏省高等学校自然科学研究项目(22KJB156);扬州市科技计划项目(YZ2022081);扬州市科技计划项目(YZ2022196);扬州工业职业技术学院自然科学类重点课题(2021xjzk004)

通讯作者: 沈明，教授，shenming@yzu.edu.cn，研究方向为功能纳米材料制备与应用

Corresponding author: SHEN Ming, Tel: 13665248181, E-mail: shenming@yzu.edu.cn

作者简介: 周慧，女，1983年生，博士

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https://www.cjmr.org/CN/10.11901/1005.3093.2023.430 或 https://www.cjmr.org/CN/Y2024/V38/I7/549

图1 前驱体和样品的合成流程示意图

图2 前驱体的SEM和TEM照片

图3 前驱体的XRD谱

图4 前驱体的XPS全谱和Bi4f、C1s和O1s的高分辨谱

表1 前驱体的元素分析结果

图5 水热时间不同的样品的SEM照片

图6 煅烧温度不同的样品的XRD谱

图7 前驱体样品的热重分析曲线

图8 280℃煅烧的Bi/β-Bi2O3异质结光催化剂的XPS全谱和Bi4f的高分辨谱

图9 在280℃煅烧的Bi/β-Bi2O3质结光催化剂的SEM、TEM图像、选区电子衍射以及HRTEM图像

图10 前驱体和Bi/β-Bi2O3样品的N2等温线(插图为其对应的孔径分布图)、纯β-Bi2O3和在280℃煅烧的Bi/β-Bi2O3样品的UV-Vis DRS谱

图11 以在280℃煅烧的Bi/β-Bi2O3为光催化剂降解LVFH溶液UV-Vis光谱时间演变曲线、不同光催化剂对LFVH降解效率曲线、其对应的准一级反应动力学拟合曲线以及以Bi/β-Bi2O3为光催化剂降解LFVH的循环实验

表2 不同光催化剂降解LVFH性能的比较

图12 以Bi/β-Bi2O3为光催化剂加入捕获剂TBA、BQ和EDTA前后降解LFVH的对比曲线以及在可见光照射下Bi、β-Bi2O3和Bi/β-Bi2O3的瞬时光电流密度

图13 在可见光照射下Bi/β-Bi2O3异质结对LVFH降解过程中光生载流子的迁移机理示意图

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