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首页> 外文学位 >Controlling the synthesis of bunte salt stabilized gold nanoparticles using a microreactor platform in concert with small angle x-ray scattering analysis.
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Controlling the synthesis of bunte salt stabilized gold nanoparticles using a microreactor platform in concert with small angle x-ray scattering analysis.

机译：使用微反应器平台与小角X射线散射分析相结合，控制丁苯橡胶盐稳定的金纳米颗粒的合成。

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摘要

Gold nanoparticles (AuNPs) have garnered considerable attention for their interesting size-dependent properties. These properties have fueled applications that span a continuum ranging from simple to sophisticated. Applications for these materials have grown more complex as syntheses for these materials have improved. For simple applications, current synthetic processes are sufficient. However, development of syntheses that generate well-defined particle sizes with specifically tailored surface functionalities is an on-going challenge for chemists. The aim of this dissertation is to improve upon current AuNP syntheses to produce sophisticated materials needed to discover new material properties, and provide efficient access to materials to develop new advanced applications. The research described in this dissertation improves upon current methods for AuNP production by using a microreactor to provide enhanced mixing and synthetic control, and small angle X-ray scattering (SAXS) as a precise, rapid, solution-based method for size distribution determination. Using four ligand-stabilized AuNP samples as reference materials, SAXS analysis was compared to traditional microscopic size determination. SAXS analysis provided similar average diameters while avoiding deposition artifacts, probing a larger number of particles, and reducing analysis time. Next, the limits of SAXS size analysis was evaluated, focusing on identifying multiple distributions in solution. Utilizing binary and ternary mixtures of well-defined AuNP reference samples, SAXS analysis was shown to be effective at identifying multiple distributions. While microscopy has limited ability to differentiate these modes, SAXS analysis is more rapid and introduces less researcher bias. Because AuNP size and ligand functionality are interdependent, accessing desired core sizes with varied functionality is challenging. To address this, a new microfluidic synthetic method was developed to produce thiolate-passivated AuNPs with targeted core sizes from 1.5 - 12 nm with tailored functionality. This ability to control size while independently varying surface functionality is unprecedented. Lastly, AuNP core formation was probed by simultaneous in situ SAXS and UV/visible spectroscopy. A coalescence mechanism for AuNP growth was observed when using Bunte salt ligands. This finding compares well to observed coalescence in other systems using weakly-passivating ligands, and supports the hypothesis that Bunte salts passivate ionically during particle growth while resulting in covalent linkages.
机译：金纳米颗粒（AuNPs）因其有趣的尺寸依赖性而备受关注。这些特性推动了从简单到复杂的整个过程的应用。随着这些材料的合成得到改善，这些材料的应用变得越来越复杂。对于简单的应用，当前的合成方法已足够。但是，开发能够产生明确定义的粒径并具有专门定制的表面功能的合成方法，对于化学家来说是一个持续的挑战。本文的目的是改进现有的AuNP合成方法，以生产发现新材料特性所需的复杂材料，并为开发新的先进应用提供有效的材料访问途径。本论文中描述的研究通过使用微反应器提供增强的混合和合成控制以及小角度X射线散射（SAXS）作为精确，快速，基于溶液的尺寸分布确定方法，对当前AuNP生产方法进行了改进。使用四个配体稳定的AuNP样品作为参考材料，将SAXS分析与传统的显微尺寸测定进行了比较。 SAXS分析提供了相似的平均直径，同时避免了沉积伪影，探测大量颗粒并减少了分析时间。接下来，评估SAXS大小分析的极限，重点是确定溶液中的多种分布。利用明确定义的AuNP参考样品的二元和三元混合物，显示出SAXS分析可有效识别多种分布。尽管显微镜分辨这些模式的能力有限，但SAXS分析速度更快，并且引入的研究者偏见也更少。由于AuNP的大小和配体的功能是相互依赖的，因此要获得具有各种功能的所需核的大小是一项挑战。为了解决这个问题，开发了一种新的微流体合成方法来生产具有目标功能的目标核心尺寸为1.5-12 nm的硫醇盐钝化的AuNP。这种在独立改变表面功能的同时控制尺寸的能力是前所未有的。最后，通过同时原位SAXS和紫外/可见光谱探测AuNP核的形成。使用Bunte盐配体时，观察到AuNP生长的聚结机制。这一发现与在使用弱钝化配体的其他系统中观察到的聚结相比较很好，并支持了这样的假说，即Bunte盐在颗粒生长过程中会发生离子钝化，同时导致共价键合。

著录项

  • 作者

    Haben, Patrick Michael.;

  • 作者单位

    University of Oregon.;

  • 授予单位 University of Oregon.;
  • 学科 Chemistry.;Inorganic chemistry.;Materials science.
  • 学位 Ph.D.
  • 年度 2013
  • 页码 215 p.
  • 总页数 215
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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