多孔棒状FeVO4的制备及可见光催化性能研究

doi:10.15541/jim20170586

无机材料学报 ›› 2018, Vol. 33 ›› Issue (9): 949-955.DOI: 10.15541/jim20170586 CSTR: 32189.14.10.15541/jim20170586

所属专题：光催化材料与技术

多孔棒状FeVO₄的制备及可见光催化性能研究

蒋海燕¹, 夏云生², 李育珍³

1. 青岛农业大学化学与药学院, 青岛 266109;
2. 渤海大学化学化工学院, 锦州 121013;
3. 太原理工大学环境科学与工程学院, 太原 030024

收稿日期:2017-12-07 修回日期:2018-02-05 出版日期:2018-09-20 网络出版日期:2018-08-14
作者简介:蒋海燕(1978-), 女, 博士研究生. E-mail: hyjiang@qau.edu.cn
基金资助:
青岛农业大学博士启动基金(663/1113317);山西省重点研发计划(一般)社会发展项目(201703D321009-5);国家自然科学基金(21676028);大学生创新创业项目(8003-02030381)

Preparation and Visible-light-driven Photocatalytic Performance of Porous Rod-like FeVO₄

JIANG Hai-Yan¹, XIA Yun-Sheng², LI Yu-Zhen³

1. College of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China;
2. College of Chemistry and Chemical Engineering, Bohai University, Jinzhou 121013, China;
3. College of Environmental Science and Engineering, Taiyuan University of Technology, Taiyuan 030024, China

Received:2017-12-07 Revised:2018-02-05 Published:2018-09-20 Online:2018-08-14
About author:JIANG Hai-Yan. E-mail: hyjiang@qau.edu.cn
Supported by:
Scientific Research Foundation of Qingdao Agricultural University (663/1113317);Shanxi Provincial Key Research and Development Plan (general) Social Development Project (201703D321009-5);National Natural Science Foundation of China (21676028);College Students Innovations Special Project Funded by Taiyuan University of Technology (8003-02030381)

摘要/Abstract

摘要：

以Fe(NO₃)₃和NH₄VO₃为无机源, 氨水为pH调节剂, 采用水热法制备了多种形貌纯三斜相的多孔FeVO₄。采用X射线衍射、扫描电子显微镜和紫外-可见漫反射光谱等技术表征了样品的物理性质。结果表明, 水热温度和反应液的pH对晶相结构和粒子形貌有较大的影响: 当水热温度为180℃, 反应液的pH为4.0或7.0时, 可制得多孔三斜相FeVO₄纳米棒; 当水热温度为120℃, 反应液的pH为4.0 时制得的三斜相FeVO₄为片状结构; 而当水热温度为180℃, 反应液的pH升至10.0或水热温度变为240℃, 反应液的pH保持4.0不变时均制得含有少量FeVO₄的Fe₂O₃。在可见光照射光催化降解甲基橙的反应中, 具有最高比表面积(10.4 m²/g)的多孔棒状FeVO₄光催化活性最高, 这是因为它具有最高的结晶度、比表面积和表面氧空位密度、多孔结构和最低的带隙能。

关键词: 多孔纳米棒, FeVO₄, 水热法, 光催化活性

Abstract:

Pure triclinic porous FeVO₄ with multiple morphologies were fabricated by adopting hydrothermal strategy using Fe(NO₃)₃ and NH₄VO₃as inorganic source and NH₃solution as pH adjuster. The samples were characterized by means of techniques such as X-ray diffraction, scanning electron microscopy, and ultraviolet-visible diffuse reflectance spectroscopy. It was found that hydrothermal temperature and pH of the precursor solution exerted a great effect on the crystalline structure and the particle morphology of the product. Porous triclinic FeVO₄ nanorods were generated hydrothermally at 180℃ and pH of 4 or 7, sheet-like FeVO₄ was obtained at pH 4.0 and hydrothermal temperature of 120℃. However, the mixture of Fe₂O₃ (in majority) and FeVO₄ (in minority) was prepared when pH of the precursor solution was raised to 10 at 180℃ or the hydrothermal temperature was raised to 240℃ at pH 4.0. Among the FeVO₄samples, porous FeVO₄ nanorods with the highest surface area of 10.4 m²/g exhibited the best visible-light-driven photocatalytic performance for the degradation of MO. It is concluded that such an excellent photocatalytic performance is attributed to its higher crystallinity, surface area, and surface oxygen vacancy density, porous structure, and lower bandgap energy.

Key words: porous nanorods, FeVO₄, hydrothermal method, photocatalytic performance

中图分类号:

TQ174

蒋海燕, 夏云生, 李育珍. 多孔棒状FeVO₄的制备及可见光催化性能研究[J]. 无机材料学报, 2018, 33(9): 949-955.

JIANG Hai-Yan, XIA Yun-Sheng, LI Yu-Zhen. Preparation and Visible-light-driven Photocatalytic Performance of Porous Rod-like FeVO₄[J]. Journal of Inorganic Materials, 2018, 33(9): 949-955.

图/表 8

图1 样品的XRD谱图

Fig. 1 XRD patterns of the samples(a) FeVO4-180-4; (b) FeVO4-180-7; (c) FeVO4-180-10; (d) FeVO4- 120-4; (e) FeVO4-240-4

图2 焙烧前FeVO4-180-4样品的TGA/DSC曲线

Fig. 2 TGA/DSC profile of the FeVO4-180-4 sample before calcinations

图3 FeVO4样品的SEM照片

Fig. 3 SEM images of the FeVO4 samples(a) FeVO4-180-4; (b) FeVO4-180-7; (c) FeVO4-120-4

图4 FeVO4样品的TEM和HRTEM照片

Fig. 4 TEM and HRTEM images of the FeVO4 samples(a) FeVO4-180-4; (b) FeVO4-180-7; (c) FeVO4-120-4

图5 FeVO4样品的(A)N2吸附-脱附等温线和(B)孔径分布曲线

Fig. 5 (A) N2 adsorption-desorption isotherms and (B) pore-size distributions of the FeVO4 samples

图6 FeVO4样品的(A) Fe2p, (B) V2p3/2, (C) O1s XPS谱图

Fig. 6 (A) Fe2p, (B) V2p3/2, and (C) O1s XPS spectra of the FeVO4 samples(a) FeVO4-180-4; (b) FeVO4-180-7; (c) FeVO4-120-4

图7 FeVO4样品的(A) 紫外-可见漫反射光谱和(B) (ahν)2随hν的变化曲线

Fig. 7 (A) UV-Vis diffuse reflectance spectra and (B) plots of the (ahν)2 versus hν of the FeVO4 samples(a) FeVO4-120-4; (b) FeVO4-180-4; (c) FeVO4-180-7

图8 在可见光(≥400 nm)照射下光催化降解甲基橙溶液过程中甲基橙浓度与可见光照射时间的关系图

Fig. 8 MO concentration versus visible-light irradiation time for the degradation of MO aqueous solution under visible-light irradiation (≥400 nm)

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多孔棒状FeVO₄的制备及可见光催化性能研究

Preparation and Visible-light-driven Photocatalytic Performance of Porous Rod-like FeVO₄

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