表面增强光谱分析用金属纳米薄膜的研制和应用
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摘要
金属纳米薄膜具有特殊的光学性质,使吸附在其表面上的分子的红外吸收得以增强,产生所谓的表面增强红外吸收(SEIRA)效应。基于此效应的表面增强红外吸收光谱(SEIRAS)是一种从分子水平上进行表面和界面分析的重要研究手段。它不仅可应用于周围环境中固-气界面的表面痕量分析,也可应用于电化学现场条件下固-液界面的吸附和反应研究。
表面增强红外光谱(SEIRAS)和表面增强拉曼光谱(SERS)是互补的姊妹光谱技术,利用两种光谱技术相结合可以获得更全面、完整的表面信息,银是应用在SEIRAS和SERS分析中最重要的金属之一,如何通过简单的方法快速、经济地在便宜的光学窗口上制备SEIRAS和SERS通用的银基底对于将银基底用于固-气界面的快速分析至关重要。本论文第一部分主要探索合理的化学沉积条件在Si片上构建用于SEIRAS和SERS常规分析用Ag纳米膜。甲醇在Pt电极上的氧化是电催化研究的重要体系,需要若干邻近Pt原子的配合才得以进行,本论文工作的第二部分内容通过在Pt电极修饰强吸附的CN~-,限制自由Pt原子数,并利用ATR-SEIRAS来研究该种修饰对Pt电氧化甲醇行为和机理的可能影响。金属纳米颗粒的形状、尺寸决定了薄膜的SEIRA效应。本论文第三部分初步研究了控制合成并组装不同尺寸、形状的金纳米颗粒,为其在SEIRAS进一步应用奠定基础。最后,本文还利用金属纳米粒子表面自组装和晶种生长法构建微流控分析用管道内壁金属层。
主要研究结果如下:
1.利用一种快捷、经济的方法将银纳米粒子沉积在Si片表面从而构建AgNP/Si(AgNP为Ag nanoparticle的缩写)基底作为表面增强红外光谱(SEIRAS)和表面增强拉曼光谱(SERS)表面痕量分析的模板。此法是将预处理Si片短时间浸泡在硝酸银和氟化氢混合溶液中,沉积Ag到Si表面的一种方法。通过试验不同浓度组合的AgNO_3和HF混合溶液确定制备SEIRAS活性基底(AgNP/Si)的合适条件,并用对硝基苯甲酸(PNBA)作为探针分子,估计出表面红外增强因子可达600。同时利用该法所制备的AgNP/Si模板应用于SERS探针分予铁原卟啉,获得了高质量的SERS图谱,同时利用优化条件下制备的基底,采用对巯基苯甲酸(PMBA)为探针分子进行SEIRAS和SERS检测,进一步表明该模板是既适用于SEIRAS又适用于SERS分析的基底。本方法有望拓展到其他金属如Au和Cu基底的制备。
2.通过利用CN~-修饰类单晶Pt纳米薄膜电极,利用CN~-限制某些反应位,并利用现场ATR-SEllLAS技术研究甲醇在CN~-修饰的具有Pt(111)优先取向的薄膜电极上电氧化过程。实验结果表明,甲醇在Pt上电氧化中间产物和Pt上的反应位分布有关。CN~-的修饰极大抑制了甲醇的电氧化,但是并未改变所谓的双路径机理,即经由CO的间接路径和经由甲酸根的直接路径,间接路径的存在。
3.对棒状金纳米粒子的合成以及组装进行了初探。利用NaBH4还原HAuCl_4得到小尺寸Au纳米粒子作为种子,在含CTAB溶液中种子生长棒状纳米粒子,其纵横比可通过改变种子与氯金酸的比例来调节。通过自组装剂(有机硅烷)或者静电吸引方法可将金纳米棒组装到红外窗口(Si)上,AFM测量表明它们在表面上保留了棒状而不发生聚集。
4.应用金属纳米粒子表面自组装和晶种生长法在毛细管道内壁生长导电性良好的金膜,金属层均匀连续、厚度可调,适合各种内径毛细管内壁金属化的快速、低成本湿法制备。
The unique optical properties of metallic nanoparticle films enable the enhancement of infrared absorption of ad-molecules,producing the so-called surface-enhanced IR absorption(SEIRA) effect.Spectroscopy based on this effect,i.e.,surface-enhanced infrared absorption spectroscopy(SEIRAS) is a powerful investigating tool for surface and interface analysis at molecular level,not only for trace analysis at solid-gas interfaces in ambient environment but also for sensitive characterization of adsorption and reaction at electrochemical solid-liquid interfaces.
First,surface-enhanced infrared absorption spectroscopy(SEIRAS) and surface-enhanced Raman scattering spectroscopy(SERS) are two complementary spectroscopic techniques,and more comprehensive surface information can be obtained by combining these two techniques.Ag is one of the most important metals used in SEIRAS and SERS analysis.It is essential to develop an economic and facile approach to fabricate both a SEIRA and SERS -active Ag substrate for its application in surface trace analysis in ambient environment.Hence,the first part of this thesis aims to seek suitable conditions for fabricating a Ag nanofilm on Si as the substrate for SERS and SEIRAS analysis.The oxidization of methanol on Pt electrode is an important system in electro-catalysis.It was believed that the participation of neighboring Pt atoms is a must. In part 2 of this thesis,a CN~--modified Pt electrode was used to limit the number of open Pt atoms accessible for methanol oxidation,and ATR-SEIRAS was utilized to investigate the behavior and mechanism of methanol electro-oxidization.Third,the SEIRA effect of metal nanofilms depends on particle sizes and shapes.Herein,Au nanoparticles with different sizes and shapes were synthesized and assembled,for potential application to SEIRAS in the near future.In addition,self-assembly and seeded growth tactics were applied to deposit continuous Au layer on the inner-wall of capillary for potential application in flow analysis.
Main achievements of this thesis are summarized as follows:
A facile and economic tactics to fabricate and immobilize silver nanoparticles on a thin Si wafer(AgNP/Si) is proposed and achieved as a "template" for SEIRAS and SERS analysis in ambient environment.The protocol involves immersion of the pretreated Si wafer in a solution containing silver nitrate and hydrofluoric acid.To screen appropriate conditions of preparing AgNP/Si for SEIRAS application,different combinations of AgNO_3 and HF concentrations were examined with para-nitrobenzoic acid(PNBA) used as the probe molecule in transmission measurements,with a maximum enhancement factor of ca.600 achieved.These SEIRA-active templates were also promising for SERS application,as demonstrated with high quality SERS spectra obtained respectively for iron(Ⅲ) protoporphyrin and para-mercaptobenzoic acid(PMBA) adlayers on AgNP/Si with the excitation line of 632.8 nm.This approach may be extended for making SEIRA and SERS-active Au and Cu nanofilms on Si.
In-situ ATR-SEIRAS was applied to investigate the process of methanol electro-oxidation on a CN~--modified Pt electrode with preferential(111) orientation where the reactive sites on Pt was partly blocked by CN~-.A coverage of 0.5 of CN~-adlayer on Pt decreased the rate of methanol electro-oxidization by an order of magnitude. Nevertheless,the dual-path mechanism,i.e.,via CO indirect path and via HCOO~- direct path,remained essentially unchanged on this surface.
Preliminary study on the controlled synthesis of gold nanorods and their self-assembly on infrared-active window has been carried out.Au seeds were prepared by the reduction of HAuCl_4 by NaBH_4,and grown in a solution containing CTAB to Au nanorods.Different aspect ratios can be tuned by varying the proportion of seeds and Au~(3+) in the solution.Electrostatic attraction of Au nanorods to SiO_2/Si substrates with and without MPTMS interlayer yielded different surface coverages of Au nanorods.AFM characterization showed that nanorods did not change their shapes upon adsorption,no aggregation was observed.
Self assembly and seeded growth tactics were utilized to deposit conductive and thickness-tunable Au layers in the inner wall of capillary,providing a convenient and economic way for metallization inside capillaries of various shapes and size.
表面增强红外光谱(SEIRAS)和表面增强拉曼光谱(SERS)是互补的姊妹光谱技术,利用两种光谱技术相结合可以获得更全面、完整的表面信息,银是应用在SEIRAS和SERS分析中最重要的金属之一,如何通过简单的方法快速、经济地在便宜的光学窗口上制备SEIRAS和SERS通用的银基底对于将银基底用于固-气界面的快速分析至关重要。本论文第一部分主要探索合理的化学沉积条件在Si片上构建用于SEIRAS和SERS常规分析用Ag纳米膜。甲醇在Pt电极上的氧化是电催化研究的重要体系,需要若干邻近Pt原子的配合才得以进行,本论文工作的第二部分内容通过在Pt电极修饰强吸附的CN~-,限制自由Pt原子数,并利用ATR-SEIRAS来研究该种修饰对Pt电氧化甲醇行为和机理的可能影响。金属纳米颗粒的形状、尺寸决定了薄膜的SEIRA效应。本论文第三部分初步研究了控制合成并组装不同尺寸、形状的金纳米颗粒,为其在SEIRAS进一步应用奠定基础。最后,本文还利用金属纳米粒子表面自组装和晶种生长法构建微流控分析用管道内壁金属层。
主要研究结果如下:
1.利用一种快捷、经济的方法将银纳米粒子沉积在Si片表面从而构建AgNP/Si(AgNP为Ag nanoparticle的缩写)基底作为表面增强红外光谱(SEIRAS)和表面增强拉曼光谱(SERS)表面痕量分析的模板。此法是将预处理Si片短时间浸泡在硝酸银和氟化氢混合溶液中,沉积Ag到Si表面的一种方法。通过试验不同浓度组合的AgNO_3和HF混合溶液确定制备SEIRAS活性基底(AgNP/Si)的合适条件,并用对硝基苯甲酸(PNBA)作为探针分子,估计出表面红外增强因子可达600。同时利用该法所制备的AgNP/Si模板应用于SERS探针分予铁原卟啉,获得了高质量的SERS图谱,同时利用优化条件下制备的基底,采用对巯基苯甲酸(PMBA)为探针分子进行SEIRAS和SERS检测,进一步表明该模板是既适用于SEIRAS又适用于SERS分析的基底。本方法有望拓展到其他金属如Au和Cu基底的制备。
2.通过利用CN~-修饰类单晶Pt纳米薄膜电极,利用CN~-限制某些反应位,并利用现场ATR-SEllLAS技术研究甲醇在CN~-修饰的具有Pt(111)优先取向的薄膜电极上电氧化过程。实验结果表明,甲醇在Pt上电氧化中间产物和Pt上的反应位分布有关。CN~-的修饰极大抑制了甲醇的电氧化,但是并未改变所谓的双路径机理,即经由CO的间接路径和经由甲酸根的直接路径,间接路径的存在。
3.对棒状金纳米粒子的合成以及组装进行了初探。利用NaBH4还原HAuCl_4得到小尺寸Au纳米粒子作为种子,在含CTAB溶液中种子生长棒状纳米粒子,其纵横比可通过改变种子与氯金酸的比例来调节。通过自组装剂(有机硅烷)或者静电吸引方法可将金纳米棒组装到红外窗口(Si)上,AFM测量表明它们在表面上保留了棒状而不发生聚集。
4.应用金属纳米粒子表面自组装和晶种生长法在毛细管道内壁生长导电性良好的金膜,金属层均匀连续、厚度可调,适合各种内径毛细管内壁金属化的快速、低成本湿法制备。
The unique optical properties of metallic nanoparticle films enable the enhancement of infrared absorption of ad-molecules,producing the so-called surface-enhanced IR absorption(SEIRA) effect.Spectroscopy based on this effect,i.e.,surface-enhanced infrared absorption spectroscopy(SEIRAS) is a powerful investigating tool for surface and interface analysis at molecular level,not only for trace analysis at solid-gas interfaces in ambient environment but also for sensitive characterization of adsorption and reaction at electrochemical solid-liquid interfaces.
First,surface-enhanced infrared absorption spectroscopy(SEIRAS) and surface-enhanced Raman scattering spectroscopy(SERS) are two complementary spectroscopic techniques,and more comprehensive surface information can be obtained by combining these two techniques.Ag is one of the most important metals used in SEIRAS and SERS analysis.It is essential to develop an economic and facile approach to fabricate both a SEIRA and SERS -active Ag substrate for its application in surface trace analysis in ambient environment.Hence,the first part of this thesis aims to seek suitable conditions for fabricating a Ag nanofilm on Si as the substrate for SERS and SEIRAS analysis.The oxidization of methanol on Pt electrode is an important system in electro-catalysis.It was believed that the participation of neighboring Pt atoms is a must. In part 2 of this thesis,a CN~--modified Pt electrode was used to limit the number of open Pt atoms accessible for methanol oxidation,and ATR-SEIRAS was utilized to investigate the behavior and mechanism of methanol electro-oxidization.Third,the SEIRA effect of metal nanofilms depends on particle sizes and shapes.Herein,Au nanoparticles with different sizes and shapes were synthesized and assembled,for potential application to SEIRAS in the near future.In addition,self-assembly and seeded growth tactics were applied to deposit continuous Au layer on the inner-wall of capillary for potential application in flow analysis.
Main achievements of this thesis are summarized as follows:
A facile and economic tactics to fabricate and immobilize silver nanoparticles on a thin Si wafer(AgNP/Si) is proposed and achieved as a "template" for SEIRAS and SERS analysis in ambient environment.The protocol involves immersion of the pretreated Si wafer in a solution containing silver nitrate and hydrofluoric acid.To screen appropriate conditions of preparing AgNP/Si for SEIRAS application,different combinations of AgNO_3 and HF concentrations were examined with para-nitrobenzoic acid(PNBA) used as the probe molecule in transmission measurements,with a maximum enhancement factor of ca.600 achieved.These SEIRA-active templates were also promising for SERS application,as demonstrated with high quality SERS spectra obtained respectively for iron(Ⅲ) protoporphyrin and para-mercaptobenzoic acid(PMBA) adlayers on AgNP/Si with the excitation line of 632.8 nm.This approach may be extended for making SEIRA and SERS-active Au and Cu nanofilms on Si.
In-situ ATR-SEIRAS was applied to investigate the process of methanol electro-oxidation on a CN~--modified Pt electrode with preferential(111) orientation where the reactive sites on Pt was partly blocked by CN~-.A coverage of 0.5 of CN~-adlayer on Pt decreased the rate of methanol electro-oxidization by an order of magnitude. Nevertheless,the dual-path mechanism,i.e.,via CO indirect path and via HCOO~- direct path,remained essentially unchanged on this surface.
Preliminary study on the controlled synthesis of gold nanorods and their self-assembly on infrared-active window has been carried out.Au seeds were prepared by the reduction of HAuCl_4 by NaBH_4,and grown in a solution containing CTAB to Au nanorods.Different aspect ratios can be tuned by varying the proportion of seeds and Au~(3+) in the solution.Electrostatic attraction of Au nanorods to SiO_2/Si substrates with and without MPTMS interlayer yielded different surface coverages of Au nanorods.AFM characterization showed that nanorods did not change their shapes upon adsorption,no aggregation was observed.
Self assembly and seeded growth tactics were utilized to deposit conductive and thickness-tunable Au layers in the inner wall of capillary,providing a convenient and economic way for metallization inside capillaries of various shapes and size.
引文
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