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In situ Time-resolved Characterization of Particle Systems in the Continuous Synthesis Process by Means of a Newly-developed USAXS/WAXS Laboratory Camera

利用新开发的 USAXS/WAXS 实验室相机对连续合成过程中的粒子系统进行原位时间分辨表征

基本信息

批准号：
262980686
负责人：
Professor Dr.-Ing. Hermann Nirschl
金额：
--
依托单位：
Arbeitsgruppe Verfahrenstechnische Maschinen (VM)
依托单位国家：
德国
项目类别：
Research Grants
财政年份：
2014
资助国家：
德国
起止时间：
2013-12-31 至 2017-12-31
项目状态：
已结题

来源：
https://gepris.dfg.de/gepris/projekt/262980686?language=en
关键词：
situ Time resolved Characterization Particle

项目摘要

Nanostructured particle systems are manufactured in many different ways and in the meantime have a high application potential due to extensive research efforts. In a continuous synthesis of nanoscale particle systems with defined properties for material-specific applications, however, it is necessary to systematically investigate the early stages of particle formation so as to better understand and control the ongoing synthesis processes, and to be able to reach the expected product properties. So far this has not yet been successfully realized for many processes as a result of enormous metrological requirements. A non-destructive measurement technique that is also suitable for liquid phases is the so-called X-ray scattering, which is very suitable for in situ process analysis. The objective of this proposed project is to develop a new ultra small- and wide-angle X-ray scattering apparatus (USAXS/WAXS) for time-resolved in situ characterization of particle systems in a continuous synthesis process. The specific modular design of the measuring system allows in situ analysis of the particle formation process by means of an appropriate adjustment of the optics to be used, the sample chamber and the measuring technique for the detection of the scattered radiation. Compared to the current state of the art, the distance between the sample and the detector can be increased by use of a corresponding X-ray optical component, resulting in an approximately 10-fold improvement in the resolution of the minimum scattering vector. Consequently, the use of the new measuring system makes it possible to analyze particulate structures with a size up to about 400 nm. Thus, the measured USAXS scattering curves provide the useful information for the structure elucidation both on the primary particle level and on the aggregate level. In addition, the simultaneous detection of the scattering curves at the wide angle enables characterization of crystal properties. The newly-developed USAXS/WAXS measuring system is intended to be tested by means of continuous synthesis of silica multiplets and core-shell magnetite-silica composites. For this purpose, an appropriate microreactor system is to be connected to the measuring cell, so that the process taking place in the particle synthesis can be studied in a time-resolved manner by adjusting the delay time. The main objective is to ensure the required product quality (particle size distribution, aggregate properties, distribution of the shell thickness, etc.) through in situ continuous monitoring and control of processes in the reacting system.

纳米结构颗粒系统以许多不同的方式制造，同时由于广泛的研究努力而具有很高的应用潜力。然而，在具有针对特定材料应用的定义特性的纳米颗粒系统的连续合成中，有必要系统地研究颗粒形成的早期阶段，以便更好地理解和控制正在进行的合成过程，并且能够达到预期的产品特性。到目前为止，由于巨大的可再生能源需求，许多工艺还没有成功地实现这一点。也适用于液相的非破坏性测量技术是所谓的X射线散射，其非常适合于现场过程分析。该项目的目标是开发一种新的超小和广角X射线散射装置（USAXS/WAXS），用于在连续合成过程中对颗粒系统进行时间分辨的原位表征。测量系统的特定模块化设计允许通过适当调整所使用的光学器件、样品室和用于检测散射辐射的测量技术来原位分析颗粒形成过程。与现有技术相比，可以通过使用相应的X射线光学组件来增加样品和检测器之间的距离，从而导致最小散射矢量的分辨率提高约10倍。因此，使用新的测量系统可以分析尺寸高达约400 nm的颗粒结构。因此，所测得的USAXS散射曲线提供了有用的信息，无论是在初级粒子水平上和聚集体水平上的结构阐明。此外，在广角散射曲线的同时检测，使晶体特性的表征。新开发的USAXS/WAXS测量系统旨在通过连续合成二氧化硅多重态和核壳型磁铁矿-二氧化硅复合材料来进行测试。为此，将适当的微反应器系统连接到测量单元，使得可以通过调节延迟时间以时间分辨的方式研究在颗粒合成中发生的过程。主要目的是确保所需的产品质量（粒度分布、骨料性能、壳厚度分布等）。通过原位连续监测和控制反应系统中的过程。