| 引用本文: | 丁秀萍,王亚斌,黄玉东.纤维状二氧化硅纳米球的水热合成与表征[J].哈尔滨工业大学学报,2018,50(2):116.DOI:10.11918/j.issn.03676234.201611111 |
| DING Xiuping,WANG Yabin,HUANG Yudong.Hydrothermal synthesis and characterization of fibrous silicananospheres[J].Journal of Harbin Institute of Technology,2018,50(2):116.DOI:10.11918/j.issn.03676234.201611111 |
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| 摘要: |
| 为了得到高比表面且尺寸均一的纤维状二氧化硅纳米球, 采用静止和搅拌水热反应法制备了该类纳米粒子, 探讨了制备机理及影响生长的因素.以同反应条件下微波法制备所得纤维状二氧化硅纳米球为参比样品, 通过扫描电镜和透射电镜(SEM和TEM)观察了微波反应法和水热反应法所得3类纤维状二氧化硅纳米球的形貌和结构特征、傅里叶变换红外光谱(FT-IR)考察了纳米粒子的化学组成、X射线衍射谱(XRD)探究了纳米粒子的体相结构信息, 以及采用氮气吸附脱附手段揭示了纳米粒子的吸附脱附类型及孔径分布.结果表明：水热反应能够生成直径较大、形貌更为均匀的纳米球; 搅拌水热反应效果更明显, 产物尺寸更为均一; 3种反应方式合成的纳米球具有相似的化学结构和化学官能团, 都属于Ⅳ型吸附且滞后环属于H3型; 3类纳米球的比表面积(和孔体积)分别为480.156 m2 /g(1.287 cm3 /g)、464.757 m2 /g(0.654 cm3 /g)和429.351 m2 /g(0.726 cm3 /g).形貌和结构的差别归因于反应体系的压力和反应母液均匀程度, 前者促使生成均匀的微乳液, 后者促进生成均匀的反胶束.
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| 关键词: 界面化学 介孔材料 二氧化硅纳米球 纤维状 乳液 |
| DOI：10.11918/j.issn.03676234.201611111 |
| 分类号:O613.7 |
| 文献标识码:A |
| 基金项目:国家自然基金面上项目(41573013)；中国科学院仪器功能开发项目(Y510171158) |
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| Hydrothermal synthesis and characterization of fibrous silicananospheres |
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DING Xiuping1,2,WANG Yabin 1,3,HUANG Yudong3
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(1.Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources(Qinghai Institute of Salt Lakes, Chinese Academy of Sciences), Xining 810008, China; 2.Salt Lake Chemistry Analysis and Test Center, Qinghai Institure of Salt Lakes, Chinese Academy of Sciences, Xining 810008, China; 3.School of Chemistry and Chemical Engineering, Harbin Institute of Technology, Harbin 150001, China)
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| Abstract: |
| To obtain high-specific-surface-area and uniform silica nanospheres of fibrous morphologies, the hydrothermal method with and without stirring was adopted to fabricate the nanoparticles, and the fabrication mechanism as well as the influencing factors on their development were explored. Taking fibrous silica nanospheres prepared by microwave method under the same condition as references, scanning electron microscope (SEM) and transmission electron microscope (TEM) were applied to observe morphologies of the silica nanospheres developed by hydrothermal and microwave methods, Fourier transform infrared spectroscopy (FT-IR) to identify chemical compositions of the three silica nanospheres, X-ray diffractometer (XRD) to reveal the crystal structures, as well as nitrogen (N2) adsorption-desorption isotherms to characterize the type of adsorption-desorption and pore diameters, respectively. The results indicate that nanospheres synthesized by hydrothermal method possess bigger sizes and more uniform morphologies. Especially, the effectiveness of hydrothermal method with stirring was more obvious. These three kinds of the as-prepared silica nanospheres own same chemical structures and chemical functional groups, and belong to Ⅳ adsorption-desorption isotherms with H3 loops. Specific surface area (and pore volumes) of the three nanospheres were 480.156 m2 /g(1.287 cm3 /g), 464.757 m2 /g(0.654 cm3 /g) and 429.351 m2 /g(0.726 cm3 /g), respectively. The pressure of the reaction system and the degree of uniformity of the reaction mother liquor collectively endow the nanospheres with special properties like morphologies and structural differences. The former accelerates uniform micellar emulsion, and the latter prompts formation of reverse micelles.
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| Key words: interface chemistry mesoporous material silica nanosphere fibrous morphology emulsion |
