三维花状结构α-FeOOH纳米材料的制备与表征

doi:10.7503/cjcu20140669

高等学校化学学报 ›› 2015, Vol. 36 ›› Issue (1): 48.doi: 10.7503/cjcu20140669

• 研究论文: 无机化学 • 上一篇下一篇

三维花状结构α-FeOOH纳米材料的制备与表征

许俊鸽¹, 李云琴¹, 苑宝玲^1,²(), 崔浩杰³, 付明来³

1. 福州大学土木工程学院, 福州 350116
2. 华侨大学土木工程学院, 厦门 361021
3. 中国科学院城市环境研究所, 厦门 361021

收稿日期:2014-07-18 修回日期:2014-12-23 出版日期:2015-01-10 发布日期:2014-12-23
作者简介:联系人简介: 苑宝玲, 女, 博士, 教授, 博士生导师, 主要从事饮用水安全保障理论与技术研究. E-mail: blyuan@hqu.edu.cn
基金资助:
国家自然科学基金(批准号: 51178117)、厦门市杰出青年科技人才创新技术项目(批准号: 3502Z20126009)和福建省自然科学基金(批准号:2012J05094)资助

Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures^†

XU Junge¹, LI Yunqin¹, YUAN Baoling^1,^2,^*(), CUI Haojie³, FU Minglai³

1. College of Civil Engineering, Fuzhou University, Fuzhou 350116, China
2. College of Civil Engineering, Huaqiao University, Xiamen 361021, China
3. Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021, China

Received:2014-07-18 Revised:2014-12-23 Online:2015-01-10 Published:2014-12-23
Contact: YUAN Baoling E-mail:blyuan@hqu.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(No.51178117), the Xiamen Natural Science Funds for Distinguished Young Scholar, China(No.3502Z20126009) and the Natural Science Foundation of Fujian, China(No.2012J05094)

摘要/Abstract

摘要：

以硫酸亚铁、尿素及乙醇为原料, 采用低温常压一步回流法制备了具有三维花状结构的α-FeOOH纳米材料. 考察了反应时间、反应温度、尿素浓度和乙醇用量对其结构和形貌的影响及α-FeOOH纳米材料对双氯芬酸钠的吸附性能. 实验结果表明, 当反应温度为90 ℃、反应时间为6 h、尿素浓度为0.1 mol/L、乙醇的体积分数为20%时, 所得α-FeOOH纳米材料具有规整的三维花状结构, 对双氯芬酸钠的吸附量达199.2 mg/g. 基于扫描电子显微镜(SEM)和X射线衍射(XRD)分析, 推断三维花状结构α-FeOOH的生长机制包括定向聚集和外延生长2个过程, 反应初期生成的高活性晶核快速形成不规则橄榄状颗粒并定向聚集成短簇状结构, 再沿z轴方向外延生长, 形成长簇的三维花状结构.

关键词: 三维花状结构, α-FeOOH, -FeOOH, 低温回流, 双氯芬酸钠, 吸附特性

Abstract:

3D flower-like α-FeOOH nanoparticles were synthesized by means of mild-temperature reflux method, and the samples were characterized via X-ray diffraction(XRD) and scanning electron microscopy(SEM). The influencing factors such as the reaction time, the reaction temperature, the concentration of urea, and the amount of ethanol were systematically investigated. The adsorption capacity of the α-FeOOH nanoparticles for diclofenac sodium was also tested. The results show that the sample prepared with 0.1 mol/L urea and 20%(volume fraction) ethanol at 90 ℃ for 6 h is in high structural uniformity with good crystal quality and has the best adsorption capactity of 199.2 mg/g for diclofenac sodium. The formation mechanism of the flower-like α-FeOOH nanostructures is involved with a combination of oriented attachment and epitaxial overgrowth. The fresh nanonuclei are formed in solution at the early reaction stage with high surface energy, then aggregate together to minimize the interfacial energy. The olive-like agglomerates orient into short clusters, continue to grow along z axis till the complete flower-like structures are formed.

Key words: 3D flower-like structure, α-FeOOH, -FeOOH, Low-temperature reflux, Diclofenac sodium, Adsorption property

中图分类号:

O614

TrendMD:

许俊鸽, 李云琴, 苑宝玲, 崔浩杰, 付明来. 三维花状结构α-FeOOH纳米材料的制备与表征. 高等学校化学学报, 2015, 36(1): 48.

XU Junge, LI Yunqin, YUAN Baoling, CUI Haojie, FU Minglai. Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures^†. Chem. J. Chinese Universities, 2015, 36(1): 48.

图/表 9

Fig.1 SEM images of the samples obtained at 0.5 h(A), 1 h(B), 2 h(C), 4 h(D), 6 h(E) and 8 h(F)

Fig.2 XRD patterns of the intermediate products obtained at 0.5(a), 1(b), 2(c), 4(d), 6(e) and 8(f)

Scheme 1 Schematic illustrations for the formation process of the flower-like α-FeOOH nanostructures

Fig.3 SEM images of the samples obtained at 70 ℃(A), 80 ℃(B) and 100 ℃(C)

Fig.4 XRD patterns of the samples obtained at 70 ℃(a), 80 ℃(b), 90 ℃(c) and 100 ℃(d)

Fig.5 SEM images of the samples obtained at different concentrations of urea c(urea)/(mol·L-1): (A) 0.05; (B) 0.2.

Fig.6 SEM images of the samples obtained with different amount of ethanol Volume fraction of ethanol: (A) 0; (B) 10%; (C) 40%.

Fig.7 N2 adsorption and desorption isotherms(A) and pore-size distribution(B) of the typical sample

Fig.8 Adsorption isotherms of diclofenac sodium using different samples a. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 90 ℃, 6 h; b. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 80 ℃, 6 h; c. c(urea): 0.1 mol/L, volume fraction of ethanol: 40%, 90 ℃, 6 h; d. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 90 ℃, 2 h.

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三维花状结构α-FeOOH纳米材料的制备与表征

Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures^†

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三维花状结构α-FeOOH纳米材料的制备与表征

Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures†

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Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures^†