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DESIGN AND DEVELOPMENT OF AN ENVIRONMENTAL CELL FOR DYNAMIC IN SITU OBSERVATION OF GAS-SOLID REACTIONS AT ELEVATED TEMPERATURES

机译:高温下气固反应动态观测环境池的设计与开发

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摘要

In situ monitoring of events in transmission electron microscopy provides information on how materials behave in their true state while varying environmental conditions (i.e. temperature and pressure) and exposure to reactant gas mixtures. In-situ results are usually different from static, post-reaction observations because they provide valuable real time - rather than post mortem - information. To facilitate applications that demand in situ observations, a transmission electron microscope specimen holder assembly has been developed in this dissertation. This assembly incorporates a gas flow and heating mechanism along with a novel window-type environmental cell. A controlled mixture of up to four different gases can be circulated through the cell during an experiment. In addition, the specimen can be heated up to a temperature of 1500 °C using a specially designed carbon dioxide laser mechanism. This heating technique provides major advantages over conventional methods in terms of product life, specimen heating time and design size. The cell design incorporates a gas reaction chamber less than 1 mm in height, enclosed between a pair of 20 nm thick silicon nitride windows. The chamber can accommodate a specimen or a grid having a diameter of 3 mm and thicknesses in the range of 50 to 100 microns. The volume for the gas environment within the chamber is approximately 3 mmc and the gas path length is less than 1 mm. This holder has been designed by incorporating cutting edge heating and MEMS technology to achieve excellent resolution along with a low thermal drift. Successful application of the holder has been shown to provide scientists with an economical alternative to dedicated transmission electron microscopes for a vast array of in situ applications. These applications include understanding the basic material properties, catalysis reactions, semiconductor device development, and nano structure fabrication.
机译:透射电子显微镜中事件的原位监测可提供有关材料如何在其真实状态下行为的信息,同时可改变环境条件(即温度和压力)以及暴露于反应气体混合物中。原位结果通常不同于静态的反应后观察结果,因为它们提供了有价值的实时信息,而不是事后检验信息。为了方便需要现场观察的应用,本文开发了一种透射电子显微镜标本架组件。该组件结合了气流和加热机制以及新型的窗式环境电池。在实验期间,最多四种不同气体的受控混合物可以循环通过电池。此外,可以使用专门设计的二氧化碳激光机构将样品加热到1500°C。就产品寿命,样品加热时间和设计尺寸而言,这种加热技术比传统方法具有主要优势。电池设计包括一个高度小于1毫米的气体反应室,该反应室围在一对20 nm厚的氮化硅窗口之间。该腔室可容纳直径为3 mm且厚度在50到100微米范围内的样本或网格。室内气体环境的体积约为3 mmc,气体路径长度小于1 mm。该支架的设计结合了最先进的加热技术和MEMS技术,可实现出色的分辨率和低热漂移。已经证明,支架的成功应用为科学家提供了一种经济实用的替代方案,可用于大量现场应用的专用透射电子显微镜。这些应用程序包括了解基本的材料特性,催化反应,半导体器件的开发以及纳米结构的制造。

著录项

  • 作者

    Deshmukh Pushkarraj Vasant;

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  • 年度 2008
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  • 原文格式 PDF
  • 正文语种 en
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