过渡金属电极/溶液界面水分子的表面增强拉曼光谱研究
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摘要
界面水的取向和构型在许多表面过程中都发挥关键的作用,并深刻影响各种界面的结构和功能,由此而长期成为表面科学、生物、化学和地质等领域的重要基础性课题。为了深入认知水在固/液界面的结构和行为,人们发展了各种原位和非原位的谱学技术,但是由于数量巨大体相(约55摩尔)的信号干扰,难以抽提出微弱的界面水信号,迄今所获得的信息尚十分有限。由于水分子的拉曼散射截面很小,常规拉曼光谱技术无法获得固/液体系的界面水的信息。表面增强拉曼光谱(SERS)由于具有检测表面分子的超高灵敏度而具有独特优势。但是,人们迄今仅在具有高SERS活性的金,银、铜电极体系获得水的SERS信号,并且难度很大,进展有限。因此,在更具应用背景的各种过渡金属(ⅧB族元素)的电极表面获得SERS信号,是一个具有重要科学意义的挑战性课题,也是本论文工作的主攻方向。
由于无法在具有弱SERS活性的铂族金属上获得水的SERS信号,我们采用了“借力”的策略,即在高SERS活性的金纳米粒子表面沉积一层极薄的过渡金属层,试图借助于金核的电磁场增强的长程作用,以获得铂和钯表面水的SERS。本论文研究的主要内容包括:(1)通过优化实验仪器条件(特别是光谱仪的收集效率),提高了实验的检测灵敏度;设计和采用立式电解池和薄层溶液技术,将研究的电位范围拓宽到有强烈氢析出的反应电位区间;(2)合成核壳结构纳米粒子,在金核表面无针孔沉积包裹极薄的铂或钯金属原子壳层,成功地在过渡金属电极表面得到了水的SERS信号,并探讨了有关电磁场增强机理。(3)为了全面认知水在各种金属表面的吸附过程和深入探讨其SERS机制,通过改变溶液的离子种类、浓度和pH值,考察了这些因素对界面水SERS行为的影响。我们比较了铂和钯基底的水的SERS谱图与金电极的明显差异,并通过量子化学计算的研究,初步提出了有关三种金属/溶液的界面水结构的模型。
The orientation and configuration of interracial water play a vital role in various surface processes and deeply influence the structure and function of different interfaces. Therefore,it has been a key fundamental issue in surface science,biology,chemistry and geology etc.for a long time.In order to completely understand the structure and behavior of water at the solid/aqueous,various in situ and ex situ techniques had been developed. However,until now the information obtained for the interfacial water is very limited because the interference from the bulk water(55 mol/L) is too severe to extract the very signal of interracial water.Normal Raman technique has a too low detection sensitivity to obtain information of the solid/aqueous interface due to the low Raman cross section of water.Surface-enhanced Raman Spectroscopy(SERS) with its ultrahigh detecting sensitivity to surface species has unique advantages over other surface techniques. However,up to now SERS of water can only be observed on silver,gold and copper with great difficulty,and the development is much slower than expected,Therefore,to obtain SERS signals of water from transition metal(ⅤⅢB group) surfaces with a wider application is a very challenging project with important scientific significance,which is the core of present thesis.
We have tried but we are unable to directly obtain SERS signal of water from Pt group metal surfaces with only weak SERS-activity.Therefore,we utilized a "borrow" strategy,i.e.,by coating a very thin transition-metal layer(Pt or Pd) over the high SERS-activity Au nanoparticles,in virtue of the long range effect of electromagnetic enhancement of Au core,to obtain the SERS signal from Pt and Pd surfaces.The main results of this thesis include:
(1) The detection sensitivity for detecting surface species was improved by optimizing experimental and instrumental conditions,especially the collecting efficiency of the instrument,including adopting suitable instrumental parameters,designing and utilizing a vertical setup of cell and thin-layer solution method.This also allows the in situ SERS investigation in the severe hydrogen evolution region.
(2) Pinhole-free Gold core thin platinum or palladium shell nanoparticles with high SERS activity were synthesized and used as substrate to successfully obtain the SERS signal of inteffacial water.A brief discussion on the on electromagnetic enhancement was made on the basis of the result modeled by 3D-FDTD calculation.
(3) For a completely understanding the process of water adsorbed on various metal surfaces and the SERS mechanism,the influence of solution pH value,the concentration of the electrolyte and the type of cations of supporting electrolyte on the structure of interfacial water was investigated.Significant difference in the SERS of water has been observed on Pt,Pd and Au surfaces.To account for the difference,a quantum chemical study was carried out and three preliminary models for water adsorbed on the three metal surfaces was proposed.
由于无法在具有弱SERS活性的铂族金属上获得水的SERS信号,我们采用了“借力”的策略,即在高SERS活性的金纳米粒子表面沉积一层极薄的过渡金属层,试图借助于金核的电磁场增强的长程作用,以获得铂和钯表面水的SERS。本论文研究的主要内容包括:(1)通过优化实验仪器条件(特别是光谱仪的收集效率),提高了实验的检测灵敏度;设计和采用立式电解池和薄层溶液技术,将研究的电位范围拓宽到有强烈氢析出的反应电位区间;(2)合成核壳结构纳米粒子,在金核表面无针孔沉积包裹极薄的铂或钯金属原子壳层,成功地在过渡金属电极表面得到了水的SERS信号,并探讨了有关电磁场增强机理。(3)为了全面认知水在各种金属表面的吸附过程和深入探讨其SERS机制,通过改变溶液的离子种类、浓度和pH值,考察了这些因素对界面水SERS行为的影响。我们比较了铂和钯基底的水的SERS谱图与金电极的明显差异,并通过量子化学计算的研究,初步提出了有关三种金属/溶液的界面水结构的模型。
The orientation and configuration of interracial water play a vital role in various surface processes and deeply influence the structure and function of different interfaces. Therefore,it has been a key fundamental issue in surface science,biology,chemistry and geology etc.for a long time.In order to completely understand the structure and behavior of water at the solid/aqueous,various in situ and ex situ techniques had been developed. However,until now the information obtained for the interfacial water is very limited because the interference from the bulk water(55 mol/L) is too severe to extract the very signal of interracial water.Normal Raman technique has a too low detection sensitivity to obtain information of the solid/aqueous interface due to the low Raman cross section of water.Surface-enhanced Raman Spectroscopy(SERS) with its ultrahigh detecting sensitivity to surface species has unique advantages over other surface techniques. However,up to now SERS of water can only be observed on silver,gold and copper with great difficulty,and the development is much slower than expected,Therefore,to obtain SERS signals of water from transition metal(ⅤⅢB group) surfaces with a wider application is a very challenging project with important scientific significance,which is the core of present thesis.
We have tried but we are unable to directly obtain SERS signal of water from Pt group metal surfaces with only weak SERS-activity.Therefore,we utilized a "borrow" strategy,i.e.,by coating a very thin transition-metal layer(Pt or Pd) over the high SERS-activity Au nanoparticles,in virtue of the long range effect of electromagnetic enhancement of Au core,to obtain the SERS signal from Pt and Pd surfaces.The main results of this thesis include:
(1) The detection sensitivity for detecting surface species was improved by optimizing experimental and instrumental conditions,especially the collecting efficiency of the instrument,including adopting suitable instrumental parameters,designing and utilizing a vertical setup of cell and thin-layer solution method.This also allows the in situ SERS investigation in the severe hydrogen evolution region.
(2) Pinhole-free Gold core thin platinum or palladium shell nanoparticles with high SERS activity were synthesized and used as substrate to successfully obtain the SERS signal of inteffacial water.A brief discussion on the on electromagnetic enhancement was made on the basis of the result modeled by 3D-FDTD calculation.
(3) For a completely understanding the process of water adsorbed on various metal surfaces and the SERS mechanism,the influence of solution pH value,the concentration of the electrolyte and the type of cations of supporting electrolyte on the structure of interfacial water was investigated.Significant difference in the SERS of water has been observed on Pt,Pd and Au surfaces.To account for the difference,a quantum chemical study was carried out and three preliminary models for water adsorbed on the three metal surfaces was proposed.
引文
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