金属微纳结构制备中多光子光化学还原过程控制研究
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摘要
金属微纳结构是指金属纳米颗粒或者金属原子/离子通过一系列物理和化学变化过程所形成的具有微米或纳米尺寸几何外形。金属微纳结构的表面等离子体效应及与之相关的应用受到人们广泛的关注。金属表面等离子体的频率和强度与金属微纳结构的几何构型、尺寸和表面形貌有密切关系,因而金属微纳结构的制备是目前研究的一个热点。然而,现在大部分的加工手段只能制备出几何构型较简单的二维结构,对于复杂三维结构的制备无能为力,这已经成为认识与三维金属纳米结构相关的新现象、新效应和新原理的巨大瓶颈,同时也极大限制了基于这些新发现的三维纳米器件的开发和应用。因此发展纳米尺度三维金属结构的重要性不言而喻。
本论文主要研究目的是解决金属微纳结构制备中多光子光化学还原过程控制问题,以制备纳米尺度的金属结构。我们通过将表面活性剂引入多光子光还原过程,限制了金属纳米颗粒的还原生长,使多光子加工技术的金属加工分辨率超过传统光学理论衍射极限,实现了纳米尺度的金属加工。同时,我们研究了加工条件对银微纳结构表面形貌、外形以及连续性的影响,揭示了在多光子过程中存在的光镊效应和激光消融效应与金属微结构形貌的关系。这对进一步研究三维金属微纳结构的光电性能以及构筑微器件具有重要意义。
本文分六章,各章具体内容如下:
第一章:本章详细介绍了相关研究背景。综述了金属纳米材料和金属微纳结构的性质和应用;概述了微纳结构不同的加工方法;详细介绍了多光子技术的原理、特点和应用,以及目前使用多光子技术加工得到的各种微纳结构。阐述了本论文所进行的研究工作的目的和意义。
第二章:本章研究了银氨络离子水溶液的光学吸收性质和在该溶液中银离子的多光子光还原特性,考察了不同激光功率、曝光时间和扫描速度对金属银微结构尺寸和表面形貌的影响,以及激光加工条件与组成银微结构的银颗粒的尺寸和形貌的关系。
第三章:本章通过将饱和脂肪酸盐表面活性剂引入多光子光还原金属银微结构的制备,研究了饱和脂肪酸盐结构对银微结构的表面形貌和尺寸的影响,发现增加脂肪酸盐碳链的长度可以促进银离子还原并可以减小银微结构的尺寸、提高表面光滑度。通过改变加工条件,考察了激光功率对银点和银线结构制备的影响,以及金属激光加工阈值的变化。通过选择合适的加工条件,银线的宽度可超越光学衍射极限。探讨表面活性剂辅助多光子光还原制备银微纳结构的机理,通过离子迁移理论计算模拟了随曝光时间增长银点结构直径的变化趋势。这些研究为进一步提高多光子金属微结构加工精度提供了基础。
第四章:本章使用表面活性剂n-癸酰肌氨酸钠盐通过多光子光还原制备一维/二维/三维金属银微纳结构,利用表面活性剂对银纳米颗粒生长的限制,使银线的宽度达到纳米尺寸,银柱的宽度接近纳米尺寸。通过调整激光加工功率和激光焦点扫描速度,来改变银微纳结构的表面形貌和外形,并进一步对银线进行溶剂和高温退火,重塑银微纳结构的形貌、改变银线的连续性。通过制作银电极和金属银光栅证明其电导性,为今后银微纳结构的光电学应用提供了参考。
第五章:本章使用多光子光还原技术在琼脂糖水凝胶中制备金属银微纳结构,研究了凝胶中各种化学物质配比对银线连续性的影响,考察了在改变加工条件下,包埋在水凝胶中的结构形态和线宽。通过比较不同的物质配比和加工条件下制备银线的形貌,分析了有利于提高银线连续性和尺寸的因素,为进一步提高水凝胶中银微结构加工精度打下了基础。
第六章:本章对本论文的研究工作和结果进行了总结,并对未来研究进行了展望。
Metallic micro/nano structures are formed through successive chemical and physical reactions of metal nanoparticles or atoms/ions, which finally achieve a shape with the geometry in micro/nano scales. These structures have attracted much attention due to their unique surface Plasmon resonance (SPR) characteristics and their SPR-related applications. Great efforts have been made concerning the fabrication of metallic micro/nano structures, due to the strong dependence of the resonance frequency and strength of the SPR on their geometry, size and surface morphology. However, most approaches are just suitable for the fabrication of simply two-dimensional (2D) structures. The lack of methods for the fabrication of three dimensional (3D) structures has greatly inhibited the new experimental finding in the research of metallic nanostructures, which also limit the potentials of 3D nano-devices applications. Therefore, it is critical important to develop the fabrication techniques for the 3D metallic nanostructures.
In this work, we focused on the fabrication of metallic nanostructure. We introduced surfactants into multiphoton induced photoreduction (MPR) process to inhibit the growth of metal particles, which led to nanometer scale fabrication exceeding the light diffraction limit. Furthermore, we investigate the dependence of surface morphologies and continuities of metallic structures on fabrication conditions. We found many unexpected effects in MPR, such as the optical tweezer, thermal and laser ablation effects, which also greatly influence morphologies of metallic structures. These researches may open the way for both the exploration of the optical/electronical properties of 3D metallic structures and the fabrication of micro/nano device in future.
The thesis contains six chapters and main points of each chapter are listed as follows:
Chapter 1: This chapter covered the background of the research. It reviewed applications and properties of metallic micro/nano structures, microfabrication methods and the principle, characteristics and applications of multiphoton microfabrication. The purpose, significance and contents were addressed in the last part.
Chapter 2: Silver microstructures were fabricated in aqueous solution by MPR. Surface morphologies and size dependence of silver structures on the laser power and exposure time was investigated. Moreover, the size and morphologies dependence of silver particles produced in MPR was also explored.
Chapter 3: Silver microstructures were fabricated in aqueous solution mixed with fatty salts by MPR. Surface morphologies and size dependence of silver structures on the chain length of fatty salts was investigated. Not only the feature size of the silver structure was reduced but also the surface smoothness was improved by increasing the chain length of the fatty salts. The threshold for the fabrication of silver structures was found by changing the laser irradiation condition. The size of silver structures can exceed the diffraction limit by optimizing the fabrication condition. Furthermore, the mechanism for surfactant assisted MPR was discussed. The dependence of the size of silver dots on the exposure time was simulated by using ions diffusion model.
Chapter 4: 1D/2D/3D silver micro/nano structures were fabricated by using n-decanoylsarcosine sodium in MPR. The smallest feature size of silver structures was in nanometer scale. The morphologies and shapes dependence of silver structures on the fabrication condition was investigated. The high temperature and solvent annealing process was also used to modify morphologies of the silver structures. In addition, the electrical conductivity of silver line was estimated by fabricating silver electrodes and silver gratings, which open the way for the investigation of the optical/electronical properties of silver micro/nano structures.
Chapter 5: Silver microstructures were fabricated in agarose gel. The morphologies and size dependence of silver structures on the ratio of reagent contents and fabrication condition was explored. The factors for improving the continuity and reducing the size of silver lines was found, which may provided the base for improving the fabrication resolution in gels.
Chapter 6: Conclusions of main research results and corresponding future researches were provided in this chapter.
本论文主要研究目的是解决金属微纳结构制备中多光子光化学还原过程控制问题,以制备纳米尺度的金属结构。我们通过将表面活性剂引入多光子光还原过程,限制了金属纳米颗粒的还原生长,使多光子加工技术的金属加工分辨率超过传统光学理论衍射极限,实现了纳米尺度的金属加工。同时,我们研究了加工条件对银微纳结构表面形貌、外形以及连续性的影响,揭示了在多光子过程中存在的光镊效应和激光消融效应与金属微结构形貌的关系。这对进一步研究三维金属微纳结构的光电性能以及构筑微器件具有重要意义。
本文分六章,各章具体内容如下:
第一章:本章详细介绍了相关研究背景。综述了金属纳米材料和金属微纳结构的性质和应用;概述了微纳结构不同的加工方法;详细介绍了多光子技术的原理、特点和应用,以及目前使用多光子技术加工得到的各种微纳结构。阐述了本论文所进行的研究工作的目的和意义。
第二章:本章研究了银氨络离子水溶液的光学吸收性质和在该溶液中银离子的多光子光还原特性,考察了不同激光功率、曝光时间和扫描速度对金属银微结构尺寸和表面形貌的影响,以及激光加工条件与组成银微结构的银颗粒的尺寸和形貌的关系。
第三章:本章通过将饱和脂肪酸盐表面活性剂引入多光子光还原金属银微结构的制备,研究了饱和脂肪酸盐结构对银微结构的表面形貌和尺寸的影响,发现增加脂肪酸盐碳链的长度可以促进银离子还原并可以减小银微结构的尺寸、提高表面光滑度。通过改变加工条件,考察了激光功率对银点和银线结构制备的影响,以及金属激光加工阈值的变化。通过选择合适的加工条件,银线的宽度可超越光学衍射极限。探讨表面活性剂辅助多光子光还原制备银微纳结构的机理,通过离子迁移理论计算模拟了随曝光时间增长银点结构直径的变化趋势。这些研究为进一步提高多光子金属微结构加工精度提供了基础。
第四章:本章使用表面活性剂n-癸酰肌氨酸钠盐通过多光子光还原制备一维/二维/三维金属银微纳结构,利用表面活性剂对银纳米颗粒生长的限制,使银线的宽度达到纳米尺寸,银柱的宽度接近纳米尺寸。通过调整激光加工功率和激光焦点扫描速度,来改变银微纳结构的表面形貌和外形,并进一步对银线进行溶剂和高温退火,重塑银微纳结构的形貌、改变银线的连续性。通过制作银电极和金属银光栅证明其电导性,为今后银微纳结构的光电学应用提供了参考。
第五章:本章使用多光子光还原技术在琼脂糖水凝胶中制备金属银微纳结构,研究了凝胶中各种化学物质配比对银线连续性的影响,考察了在改变加工条件下,包埋在水凝胶中的结构形态和线宽。通过比较不同的物质配比和加工条件下制备银线的形貌,分析了有利于提高银线连续性和尺寸的因素,为进一步提高水凝胶中银微结构加工精度打下了基础。
第六章:本章对本论文的研究工作和结果进行了总结,并对未来研究进行了展望。
Metallic micro/nano structures are formed through successive chemical and physical reactions of metal nanoparticles or atoms/ions, which finally achieve a shape with the geometry in micro/nano scales. These structures have attracted much attention due to their unique surface Plasmon resonance (SPR) characteristics and their SPR-related applications. Great efforts have been made concerning the fabrication of metallic micro/nano structures, due to the strong dependence of the resonance frequency and strength of the SPR on their geometry, size and surface morphology. However, most approaches are just suitable for the fabrication of simply two-dimensional (2D) structures. The lack of methods for the fabrication of three dimensional (3D) structures has greatly inhibited the new experimental finding in the research of metallic nanostructures, which also limit the potentials of 3D nano-devices applications. Therefore, it is critical important to develop the fabrication techniques for the 3D metallic nanostructures.
In this work, we focused on the fabrication of metallic nanostructure. We introduced surfactants into multiphoton induced photoreduction (MPR) process to inhibit the growth of metal particles, which led to nanometer scale fabrication exceeding the light diffraction limit. Furthermore, we investigate the dependence of surface morphologies and continuities of metallic structures on fabrication conditions. We found many unexpected effects in MPR, such as the optical tweezer, thermal and laser ablation effects, which also greatly influence morphologies of metallic structures. These researches may open the way for both the exploration of the optical/electronical properties of 3D metallic structures and the fabrication of micro/nano device in future.
The thesis contains six chapters and main points of each chapter are listed as follows:
Chapter 1: This chapter covered the background of the research. It reviewed applications and properties of metallic micro/nano structures, microfabrication methods and the principle, characteristics and applications of multiphoton microfabrication. The purpose, significance and contents were addressed in the last part.
Chapter 2: Silver microstructures were fabricated in aqueous solution by MPR. Surface morphologies and size dependence of silver structures on the laser power and exposure time was investigated. Moreover, the size and morphologies dependence of silver particles produced in MPR was also explored.
Chapter 3: Silver microstructures were fabricated in aqueous solution mixed with fatty salts by MPR. Surface morphologies and size dependence of silver structures on the chain length of fatty salts was investigated. Not only the feature size of the silver structure was reduced but also the surface smoothness was improved by increasing the chain length of the fatty salts. The threshold for the fabrication of silver structures was found by changing the laser irradiation condition. The size of silver structures can exceed the diffraction limit by optimizing the fabrication condition. Furthermore, the mechanism for surfactant assisted MPR was discussed. The dependence of the size of silver dots on the exposure time was simulated by using ions diffusion model.
Chapter 4: 1D/2D/3D silver micro/nano structures were fabricated by using n-decanoylsarcosine sodium in MPR. The smallest feature size of silver structures was in nanometer scale. The morphologies and shapes dependence of silver structures on the fabrication condition was investigated. The high temperature and solvent annealing process was also used to modify morphologies of the silver structures. In addition, the electrical conductivity of silver line was estimated by fabricating silver electrodes and silver gratings, which open the way for the investigation of the optical/electronical properties of silver micro/nano structures.
Chapter 5: Silver microstructures were fabricated in agarose gel. The morphologies and size dependence of silver structures on the ratio of reagent contents and fabrication condition was explored. The factors for improving the continuity and reducing the size of silver lines was found, which may provided the base for improving the fabrication resolution in gels.
Chapter 6: Conclusions of main research results and corresponding future researches were provided in this chapter.
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