离子液体辅助下贵金属纳米材料的制备
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摘要
纳米材料是纳米科技应用的基础,贵金属纳米粒子尤其是Au、Ag纳米微粒的尺寸和形貌控制以及相应的物理化学性质一直是纳米材料科学研究的热点。离子液体作为一种新型的“绿色化学产品”,受到了众多科研工作者的广泛关注。近年来,在离子液体辅助下制备纳米材料的报道已有出现。离子液体的较低界面张力和超分子自组装能力可为纳米材料的制备提供新的方法。本论文将离子液体的这两种作用应用于贵金属纳米材料的制备中,首先,在少量的咪唑型短链离子液体辅助下,通过乙二醇法制备出Ag纳米棒；之后,在短链和长链离子液体共同辅助下,制备了Au和Pt的纳米花状物。论文的具体内容如下：
第一章从纳米材料和离子液体的概念入手,对它们的研究现状进行了概述。之后又简要介绍了国内外关于在离子液体辅助下制备贵金属纳米材料的研究背景,为论文的研究提供了理论依据。最后,阐述了本论文选题的科学意义。
第二章系统地研究了在少量短链离子液体1-丁基-3-甲基咪唑四氟硼酸盐(bmimBF4辅助下,在130℃通过乙二醇还原得到了Ag纳米棒。首先,通过扫描电镜(SEM)和透射电镜(TEM)确定了产物的形貌和纯度。又用高分辨电镜(HRTEM)和电子衍射(ED)证明了产物的生长方向。然后,结合时间和其它辅助剂对产物的影响,确定了产物的形成机理。结果表明银纳米棒是由五重挛晶结构的纳米颗粒沿(111)面生长形成的。实验证实离子液体的较低界面张力可促使小颗粒通过奥氏熟化快速形成,离子液体在实验中起着不可或缺的作用。在此基础上,将原来的两步反应简化为一步反应,大大缩短了反应时间,但也同样得到了形貌和尺寸均一的银纳米棒。还研究了产物的光学性能,紫外可见光谱的表征证实Ag纳米棒具有良好的表面增强的等离子共振(SPR)性质。此外,我们选用R6G为探针分子研究了Ag纳米棒形成的自组装膜作为表面增强的拉曼散射(SERS)基底的增强效应,结果表明即使R6G的浓度非常低,使用Ag纳米棒自组装膜基底仍能够探测到在一般拉曼谱图中无法探测的信号。
第三章研究了在短链离子液体bmimBF4和长链离子液体C12mimBr共同辅助下,制备出Au和Pt的纳米花状物。通过扫描电镜(SEM)和透射电镜(TEM)对产物的形貌进行了表征。又通过电子能谱仪(EDS)确定了产物的纯度。电子衍射(ED)确定了产物的晶型。结果表明,花状产物是由纳米板自组装形成的,离子液体bmimBF4的咪唑环之间的π-π堆积作用是纳米板进行自组装的基础。此外,两种离子液体C12mimBr和bmimBF4的质量比对纳米花状物的形成有着决定性的影响。
Nanomaterials were the base of the application of nanotechnology. The synthesis of noble metal nanostructured materials especially Au, Ag nanoparticles with controllable size and morphology was always attractive in the field of nanomaterials. As a "green" chemical product, ionic liquids (ILs) have currently attracted significant attention. Recently, the preparation of nanomaterials with the assistance of ILs was reported in the literature. The lower interface tensions and supramolecular self-assembly of ILs provide new methods for the synthesis of nanomaterials. In this dissertation, we prepared silver nanorods through ethylene glycol (EG) reduction in the presence of imidazole-based ionic liquid (IL) and polyvinyl pyrrolidone (PVP). In addition, with the assistance of short-chain and long-chain ILs, the flower-like nanomaterials of Au and Pt were synthesized. The outline and contents of this dissertation were as follows:
Chapter one was a brief introduction of the research background of this work, in which a review of nanomaterials and ILs are present, and then the history and recent progress in the preparation of nanomaterials associated with ILs are reviewed. The objective and the scientific significance of this dissertation were also pointed out at the end of this part.
In Chapter two, the preparation of silver nanorods in the presence of IL 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4) was investigated in detail. First, the shape of products was conformed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Then the growth direction was verified through the high resolution transmission electron microscope (HRTEM) and electron diffraction (ED). The formation mechanism was investigated by exploring the influence of time and other modulators on the products. The results demonstrated that the silver nanrods evolved from multiply twinned nanoparticles with a decahedral shape along (111) facet. Low interface tensions of bmimBF4 result in high nucleation rates, very small particles can be generated which undergo Ostwald ripening. BmimBF4 played a crucial role in the process. Moreover, the synthesis process was simplified to a "one-step reaction", and the reaction time was shortened to three hours. The products were silver nanorods with uniform dimension and shape all the same. The optical property of nanorods was investigated by UV-Vis spectra. The results showed silver nanorods possessed well surface plasmon resonance (SPR). Whats more, the surface-enhanced Raman scattering (SERS) of self-assembled silver nanorod array film with the Rhodamine 6G (R6G) as the probe molecule was also investigated. The results demonstrated that using the array film substrate could detect SERS signal of R6G even that the concentration of R6G was very low.
In chapter three, the synthesis of flower-like Au/Pt nanomaterials in the presence of ILs 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4) and 1-dodecyl-3-methylimidazolium bromide (C12mimBr) was investigated. The dimension and morphology of the products were characterized by SEM and TEM. The purity was confirmed by electron energy disperse spectroscopy (EDS). The crystal was proved by electron diffraction (ED). The results demonstrated that flower-like nanomaterials were formed by self-assembled nanoplates. This self-assembly process was supported byπ-πstack interaction of the neighboring imidazolium rings of bmimBF4. Furthermore, the mass ratio between C12mimBr and bmimBF4 played an important role in the formation process.
第一章从纳米材料和离子液体的概念入手,对它们的研究现状进行了概述。之后又简要介绍了国内外关于在离子液体辅助下制备贵金属纳米材料的研究背景,为论文的研究提供了理论依据。最后,阐述了本论文选题的科学意义。
第二章系统地研究了在少量短链离子液体1-丁基-3-甲基咪唑四氟硼酸盐(bmimBF4辅助下,在130℃通过乙二醇还原得到了Ag纳米棒。首先,通过扫描电镜(SEM)和透射电镜(TEM)确定了产物的形貌和纯度。又用高分辨电镜(HRTEM)和电子衍射(ED)证明了产物的生长方向。然后,结合时间和其它辅助剂对产物的影响,确定了产物的形成机理。结果表明银纳米棒是由五重挛晶结构的纳米颗粒沿(111)面生长形成的。实验证实离子液体的较低界面张力可促使小颗粒通过奥氏熟化快速形成,离子液体在实验中起着不可或缺的作用。在此基础上,将原来的两步反应简化为一步反应,大大缩短了反应时间,但也同样得到了形貌和尺寸均一的银纳米棒。还研究了产物的光学性能,紫外可见光谱的表征证实Ag纳米棒具有良好的表面增强的等离子共振(SPR)性质。此外,我们选用R6G为探针分子研究了Ag纳米棒形成的自组装膜作为表面增强的拉曼散射(SERS)基底的增强效应,结果表明即使R6G的浓度非常低,使用Ag纳米棒自组装膜基底仍能够探测到在一般拉曼谱图中无法探测的信号。
第三章研究了在短链离子液体bmimBF4和长链离子液体C12mimBr共同辅助下,制备出Au和Pt的纳米花状物。通过扫描电镜(SEM)和透射电镜(TEM)对产物的形貌进行了表征。又通过电子能谱仪(EDS)确定了产物的纯度。电子衍射(ED)确定了产物的晶型。结果表明,花状产物是由纳米板自组装形成的,离子液体bmimBF4的咪唑环之间的π-π堆积作用是纳米板进行自组装的基础。此外,两种离子液体C12mimBr和bmimBF4的质量比对纳米花状物的形成有着决定性的影响。
Nanomaterials were the base of the application of nanotechnology. The synthesis of noble metal nanostructured materials especially Au, Ag nanoparticles with controllable size and morphology was always attractive in the field of nanomaterials. As a "green" chemical product, ionic liquids (ILs) have currently attracted significant attention. Recently, the preparation of nanomaterials with the assistance of ILs was reported in the literature. The lower interface tensions and supramolecular self-assembly of ILs provide new methods for the synthesis of nanomaterials. In this dissertation, we prepared silver nanorods through ethylene glycol (EG) reduction in the presence of imidazole-based ionic liquid (IL) and polyvinyl pyrrolidone (PVP). In addition, with the assistance of short-chain and long-chain ILs, the flower-like nanomaterials of Au and Pt were synthesized. The outline and contents of this dissertation were as follows:
Chapter one was a brief introduction of the research background of this work, in which a review of nanomaterials and ILs are present, and then the history and recent progress in the preparation of nanomaterials associated with ILs are reviewed. The objective and the scientific significance of this dissertation were also pointed out at the end of this part.
In Chapter two, the preparation of silver nanorods in the presence of IL 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4) was investigated in detail. First, the shape of products was conformed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Then the growth direction was verified through the high resolution transmission electron microscope (HRTEM) and electron diffraction (ED). The formation mechanism was investigated by exploring the influence of time and other modulators on the products. The results demonstrated that the silver nanrods evolved from multiply twinned nanoparticles with a decahedral shape along (111) facet. Low interface tensions of bmimBF4 result in high nucleation rates, very small particles can be generated which undergo Ostwald ripening. BmimBF4 played a crucial role in the process. Moreover, the synthesis process was simplified to a "one-step reaction", and the reaction time was shortened to three hours. The products were silver nanorods with uniform dimension and shape all the same. The optical property of nanorods was investigated by UV-Vis spectra. The results showed silver nanorods possessed well surface plasmon resonance (SPR). Whats more, the surface-enhanced Raman scattering (SERS) of self-assembled silver nanorod array film with the Rhodamine 6G (R6G) as the probe molecule was also investigated. The results demonstrated that using the array film substrate could detect SERS signal of R6G even that the concentration of R6G was very low.
In chapter three, the synthesis of flower-like Au/Pt nanomaterials in the presence of ILs 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF4) and 1-dodecyl-3-methylimidazolium bromide (C12mimBr) was investigated. The dimension and morphology of the products were characterized by SEM and TEM. The purity was confirmed by electron energy disperse spectroscopy (EDS). The crystal was proved by electron diffraction (ED). The results demonstrated that flower-like nanomaterials were formed by self-assembled nanoplates. This self-assembly process was supported byπ-πstack interaction of the neighboring imidazolium rings of bmimBF4. Furthermore, the mass ratio between C12mimBr and bmimBF4 played an important role in the formation process.
引文
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