基于纳米结构表面增强拉曼散射的近场光谱学与掩埋分子体系研究
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摘要
表面增强拉曼散射(SERS)效应可以极大地增强吸附在特定金属纳米结构表面的分子(离子)的拉曼散射强度,因而较为广泛地应用于电化学等界面科学和分析科学研究领域。为了全面发展表面增强拉曼光谱学和进一步拓宽其应用体系,需要从更深的层次全面认识SERS机理。
SERS效应作为纳米尺度下所具有的特殊光学效应而与纳米科学有密切的联系,作为激光、分子和纳米结构三者相互联系的综合体而包含着深刻的物理和化学规律。然而,传统的SERS研究往往只关注于SERS光谱所表现出的宏观图像和平均信息,而忽略了从SERS信号所发生的纳米尺度之下对固体表面纳米结构与分子之间的相互作用进行研究,进而在微观尺度之下更客观而具体地对SERS现象的本质进行分析。因此,SERS现象和机理的研究需要发展在纳米体系下的检测方法和样品制备方法,并应在研究过程中引入更多新型的纳米结构体系。基于这个想法,本论文工作主要在以下几个方面开展研究,并取得如下成果:
1)将硅悬臂梁型近场光学显微镜(SNOM)与SERS光谱技术相结合,发展和改进了近场SERS光谱及成像技术。由于SNOM与SERS的结合在技术上将面临很多实际困难,例如近场激发信号极其微弱、纳米级微弱光谱的收集对实验精度和环境稳定性的苛刻要求等,因此我们对实验体系和仪器工作状态分别进行了优化。
2)获得了银纳米粒子SERS基底上[Ru(Bpy)_3]~(2+)分子在纳米尺度下的近场SERS光谱和图像,从中可以发现一些近场SERS效应特有的现象:通过观察不同位置得到的近场SERS光谱可以发现,在纳米尺度下,由于分子所处局域环境不同而体现出不同的光谱特征;此基底具有极高SERS活性的位点(热点)远多于表面增强荧光(SEF)热点,且两者的分布并不完全一致。这可能是由多种因素的共同影响产生的结果,这些因素包括:SERS与SEF不同的增强效率、来自针尖和基底的淬灭作用,以及产生SERS和SEF效应的分子数量不同。
3)通过比较[Ru(Bpy)_3]~(2+)分子的近场与远场SERS谱图可以发现几种差异:近场SERS谱的峰位置随时间可发生变化。这可能主要是由于位于纳米结构间隙处局域化且无规则的不同的分子吸附态引起的;在532 nm激光激发下,远场SERS谱体现出的是典型的共振拉曼光谱,而近场SERS光谱体现出的则是典型的非共振拉曼光谱。这可能是由于近场的电场梯度效应和针尖小孔处激光各向异性的极化引起的;近砈ERS谱图中一些强峰的峰位置相对于远场SERS谱出现了蓝移。这可能是由于远场与近场不同的激发方式导致了分子振动能级之间的微小差异,从而引起峰位置的微小位移;从某些近场SERS光谱中可以观察到包括两个IR活性振动峰在内的三个远场SERS谱图中没有的峰。这可以解释为电场梯度效应,以及激发态配体阴离子的存在。
4)分别对银纳米粒子基底上PATP以及R6G分子的近场光谱和图像进行了初步研究.从实验可以观察到这两种分子的近场SERS和SEF强度随近场激发光强度变化的关系;通过比较以PATP不同振动峰所得到的近场SERS图像可以看到,不同的振动模在近场下具有相同的强度变化趋势;将R6G与银纳米粒子用粒子上的保护剂隔开,可以得到R6G的近场SEF图像,由图像可发现近场SEF的热点分布在粒子间隙之间具有较强局域电磁场集中的区域。此外,还将不同扫描条件对的AFM图像的影响进行了初步探讨。
5)较为系统地对探针分子埋覆于金膜之下的BM-SERS(Buried Molecule-SERS)体系进行了研究。表面金膜以不同的形式进行了纳米级粗糙,因而这种BM-SERS纳米结构是一种较为新颖的SERS研究体系。首先改变最外层金属厚度和样品的结构,利用Pb-UPD、电位阶跃、循环伏安、分子取代、改变pH值、变温原位SERS、XPS等方法证实了探针分子确实可以在真空溅射的过程中埋覆于表面金膜之下,然后再利用电化学原位SERS、理论计算等不同的方法对BM-SERS体系SERS增强产生的电荷转移(CT)机理进行研究。
The surface-enhanced Raman scattering (SERS) effect can prodigiously enhance the Raman scattering intensity of molecules (ions) adsorbed onto the surface of metal nano-structures. Therefore, it is broadly applied in the research fields of the interface sciences, such as electrochemistry, and analytical science. In order to fully develop surface-enhanced Raman spectroscopy and further broaden its application system, a comprehensive understanding of the SERS mechanisms is required.
As a special optical effect at the nano-scale range, SERS effect is closely related with nano-science. As the syntheses of the laser, molecule and nano-structure, it involves profound rules for physics and chemistry. Nevertheless, the traditional studies on SERS are mostly focused on the macroscopic views and averaged information of SERS spectroscopy. Thus, the studies on the interaction between the nano-structure and molecules on the solid surface from the SERS signal at nano-scale and the external and idiographic analysis of the hypostasis of the SERS phenomenon are usually ignored. As a consequence, to obtain better understanding for SERS phenomenon and mechanisms, it is very necessary to develop new methods for probing at nano-scale level and new methods for the preparation of nano-structure samples. Furthermore, the new nano-structure systems in different styles should be induced in the investigation process. Based on these expects, this thesis mainly focuses on the following areas to study and obtained the following results:
1) Jointing the techniques of cantilever-type scanning near-field optical microscopy (SNOM) and SERS, and the near-field SERS spectroscopy and imaging technique were developed and improved. The combination of SNOM and SERS would have many practical difficulties technically. For example, the near-field excitation signal is extremely weak, the critical environmental requirements of precision and stability for the collection of weak nano-scale spectra. Therefore we have optimized the experimental system and the working status of instrument.
2) The near-field SERS spectra and images for the [Ru(Bpy)_3]~(2+) molecule adsorbed on silver nanoparticle substrate were achieved. Based on the results, some specific phenomena for near-field SERS were found. By observing the near-field SERS spectra collected at different location at the nano-scale, the different spectral characteristics which are caused by the local environmental differences of molecules have been found. On the substrate, the highly SERS active sites (hot spots) are much more than SEF hot spots, and the distribution of them is not entirely consistent. This phenomenon could be explained by the influences of several factors including the different enhancement efficiencies existed for SERS and SEF, the quenching effects for fluorescence by the metal substrate and metal-coated tip, and the presence of different numbers of probing molecules in SERS and SEF.
3) It is of interest that the near-field and far-field SER spectra demonstrate several distinctively different spectral features. The peak wavenumber in the near-field spectra is not as stable as those of the far-field spectra. This could be mainly due to the different molecular adsorption states within the small but irregular nanoparticle junctions. When excited by 532 nm laser, the far-field SER spectrum represents a typical resonance Raman spectrum whereas the near-field SER spectral behaves like the far-field non-resonance Raman spectrum. We tried to figure out this abnormal phenomenon by the electric field gradient effect in the near-field, and the heterogeneous polarization of output laser from the tip aperture. It can be found that the main bands in near-field SERS spectrum are blue-shifted compared with the far-field SERS bands. This may due to the different excitation methods between near-field and far-field induced slight difference between the energy levels, thus leading to the small displacements. The observation of some extra bands including the IR active bands in the near-field SERS was accounted for also by the electric field gradient effect, and the existence of excited state bpy~- anion.
4) The near-field spectroscopic and imaging studies of PATP and R6G molecules adsorbed on silver nanoparticles-coated substrates were preliminarily investigated. The relationship of the near-field SERS or SEF intensities of two molecules with the incident near-field light intensity can be obtained from the experimental results. After comparison of the near-field images which are derived from different vibrational modes, it can be found that the intensity changing trends are the same for these modes. When the probe molecules of R6G are separated from silver nanopartiles with protecting agent, the near-field SEF image of R6G can be obtained. It can be found that the SEF hot spots are distributed at the junction positions between particles where stronger electromagnetic fields were located. In addition, the effects of different scanning conditions on AFM imaging quality were preliminary discussed.
5) The buried-SERS of the probe molecules buried beneath the outermost gold film was systematically investigated. The top gold films were roughed by different methods, therefore the BM-SERS (Buried Molecule-SERS) nano-structure system can be considered as a kind of novel SERS system. Firstly, after the thickness of the surface gold layers were changed, the results of the Pb-UPD, potential step method, cyclic voltammetry, molecular replacement, pH changing, temperature in-situ SERS, XPS etc. demonstrated that the probe molecules can be really buried by the metal atoms while vacuum sputtering process. Afterwards, the mechanism of the charge transfer induced with the SERS of the BM-SERS system can be investigated with the electrochemical in-situ SERS, theory calculations etc. methods.
SERS效应作为纳米尺度下所具有的特殊光学效应而与纳米科学有密切的联系,作为激光、分子和纳米结构三者相互联系的综合体而包含着深刻的物理和化学规律。然而,传统的SERS研究往往只关注于SERS光谱所表现出的宏观图像和平均信息,而忽略了从SERS信号所发生的纳米尺度之下对固体表面纳米结构与分子之间的相互作用进行研究,进而在微观尺度之下更客观而具体地对SERS现象的本质进行分析。因此,SERS现象和机理的研究需要发展在纳米体系下的检测方法和样品制备方法,并应在研究过程中引入更多新型的纳米结构体系。基于这个想法,本论文工作主要在以下几个方面开展研究,并取得如下成果:
1)将硅悬臂梁型近场光学显微镜(SNOM)与SERS光谱技术相结合,发展和改进了近场SERS光谱及成像技术。由于SNOM与SERS的结合在技术上将面临很多实际困难,例如近场激发信号极其微弱、纳米级微弱光谱的收集对实验精度和环境稳定性的苛刻要求等,因此我们对实验体系和仪器工作状态分别进行了优化。
2)获得了银纳米粒子SERS基底上[Ru(Bpy)_3]~(2+)分子在纳米尺度下的近场SERS光谱和图像,从中可以发现一些近场SERS效应特有的现象:通过观察不同位置得到的近场SERS光谱可以发现,在纳米尺度下,由于分子所处局域环境不同而体现出不同的光谱特征;此基底具有极高SERS活性的位点(热点)远多于表面增强荧光(SEF)热点,且两者的分布并不完全一致。这可能是由多种因素的共同影响产生的结果,这些因素包括:SERS与SEF不同的增强效率、来自针尖和基底的淬灭作用,以及产生SERS和SEF效应的分子数量不同。
3)通过比较[Ru(Bpy)_3]~(2+)分子的近场与远场SERS谱图可以发现几种差异:近场SERS谱的峰位置随时间可发生变化。这可能主要是由于位于纳米结构间隙处局域化且无规则的不同的分子吸附态引起的;在532 nm激光激发下,远场SERS谱体现出的是典型的共振拉曼光谱,而近场SERS光谱体现出的则是典型的非共振拉曼光谱。这可能是由于近场的电场梯度效应和针尖小孔处激光各向异性的极化引起的;近砈ERS谱图中一些强峰的峰位置相对于远场SERS谱出现了蓝移。这可能是由于远场与近场不同的激发方式导致了分子振动能级之间的微小差异,从而引起峰位置的微小位移;从某些近场SERS光谱中可以观察到包括两个IR活性振动峰在内的三个远场SERS谱图中没有的峰。这可以解释为电场梯度效应,以及激发态配体阴离子的存在。
4)分别对银纳米粒子基底上PATP以及R6G分子的近场光谱和图像进行了初步研究.从实验可以观察到这两种分子的近场SERS和SEF强度随近场激发光强度变化的关系;通过比较以PATP不同振动峰所得到的近场SERS图像可以看到,不同的振动模在近场下具有相同的强度变化趋势;将R6G与银纳米粒子用粒子上的保护剂隔开,可以得到R6G的近场SEF图像,由图像可发现近场SEF的热点分布在粒子间隙之间具有较强局域电磁场集中的区域。此外,还将不同扫描条件对的AFM图像的影响进行了初步探讨。
5)较为系统地对探针分子埋覆于金膜之下的BM-SERS(Buried Molecule-SERS)体系进行了研究。表面金膜以不同的形式进行了纳米级粗糙,因而这种BM-SERS纳米结构是一种较为新颖的SERS研究体系。首先改变最外层金属厚度和样品的结构,利用Pb-UPD、电位阶跃、循环伏安、分子取代、改变pH值、变温原位SERS、XPS等方法证实了探针分子确实可以在真空溅射的过程中埋覆于表面金膜之下,然后再利用电化学原位SERS、理论计算等不同的方法对BM-SERS体系SERS增强产生的电荷转移(CT)机理进行研究。
The surface-enhanced Raman scattering (SERS) effect can prodigiously enhance the Raman scattering intensity of molecules (ions) adsorbed onto the surface of metal nano-structures. Therefore, it is broadly applied in the research fields of the interface sciences, such as electrochemistry, and analytical science. In order to fully develop surface-enhanced Raman spectroscopy and further broaden its application system, a comprehensive understanding of the SERS mechanisms is required.
As a special optical effect at the nano-scale range, SERS effect is closely related with nano-science. As the syntheses of the laser, molecule and nano-structure, it involves profound rules for physics and chemistry. Nevertheless, the traditional studies on SERS are mostly focused on the macroscopic views and averaged information of SERS spectroscopy. Thus, the studies on the interaction between the nano-structure and molecules on the solid surface from the SERS signal at nano-scale and the external and idiographic analysis of the hypostasis of the SERS phenomenon are usually ignored. As a consequence, to obtain better understanding for SERS phenomenon and mechanisms, it is very necessary to develop new methods for probing at nano-scale level and new methods for the preparation of nano-structure samples. Furthermore, the new nano-structure systems in different styles should be induced in the investigation process. Based on these expects, this thesis mainly focuses on the following areas to study and obtained the following results:
1) Jointing the techniques of cantilever-type scanning near-field optical microscopy (SNOM) and SERS, and the near-field SERS spectroscopy and imaging technique were developed and improved. The combination of SNOM and SERS would have many practical difficulties technically. For example, the near-field excitation signal is extremely weak, the critical environmental requirements of precision and stability for the collection of weak nano-scale spectra. Therefore we have optimized the experimental system and the working status of instrument.
2) The near-field SERS spectra and images for the [Ru(Bpy)_3]~(2+) molecule adsorbed on silver nanoparticle substrate were achieved. Based on the results, some specific phenomena for near-field SERS were found. By observing the near-field SERS spectra collected at different location at the nano-scale, the different spectral characteristics which are caused by the local environmental differences of molecules have been found. On the substrate, the highly SERS active sites (hot spots) are much more than SEF hot spots, and the distribution of them is not entirely consistent. This phenomenon could be explained by the influences of several factors including the different enhancement efficiencies existed for SERS and SEF, the quenching effects for fluorescence by the metal substrate and metal-coated tip, and the presence of different numbers of probing molecules in SERS and SEF.
3) It is of interest that the near-field and far-field SER spectra demonstrate several distinctively different spectral features. The peak wavenumber in the near-field spectra is not as stable as those of the far-field spectra. This could be mainly due to the different molecular adsorption states within the small but irregular nanoparticle junctions. When excited by 532 nm laser, the far-field SER spectrum represents a typical resonance Raman spectrum whereas the near-field SER spectral behaves like the far-field non-resonance Raman spectrum. We tried to figure out this abnormal phenomenon by the electric field gradient effect in the near-field, and the heterogeneous polarization of output laser from the tip aperture. It can be found that the main bands in near-field SERS spectrum are blue-shifted compared with the far-field SERS bands. This may due to the different excitation methods between near-field and far-field induced slight difference between the energy levels, thus leading to the small displacements. The observation of some extra bands including the IR active bands in the near-field SERS was accounted for also by the electric field gradient effect, and the existence of excited state bpy~- anion.
4) The near-field spectroscopic and imaging studies of PATP and R6G molecules adsorbed on silver nanoparticles-coated substrates were preliminarily investigated. The relationship of the near-field SERS or SEF intensities of two molecules with the incident near-field light intensity can be obtained from the experimental results. After comparison of the near-field images which are derived from different vibrational modes, it can be found that the intensity changing trends are the same for these modes. When the probe molecules of R6G are separated from silver nanopartiles with protecting agent, the near-field SEF image of R6G can be obtained. It can be found that the SEF hot spots are distributed at the junction positions between particles where stronger electromagnetic fields were located. In addition, the effects of different scanning conditions on AFM imaging quality were preliminary discussed.
5) The buried-SERS of the probe molecules buried beneath the outermost gold film was systematically investigated. The top gold films were roughed by different methods, therefore the BM-SERS (Buried Molecule-SERS) nano-structure system can be considered as a kind of novel SERS system. Firstly, after the thickness of the surface gold layers were changed, the results of the Pb-UPD, potential step method, cyclic voltammetry, molecular replacement, pH changing, temperature in-situ SERS, XPS etc. demonstrated that the probe molecules can be really buried by the metal atoms while vacuum sputtering process. Afterwards, the mechanism of the charge transfer induced with the SERS of the BM-SERS system can be investigated with the electrochemical in-situ SERS, theory calculations etc. methods.
引文
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