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.

纳米结构的粒子系统以许多不同的方式制造，并且由于广泛的研究工作，因此具有很高的应用潜力。然而，在具有针对特定于材料的应用具有定义特性的纳米级粒子系统的连续合成中，有必要系统地研究粒子形成的早期阶段，以更好地理解和控制正在进行的合成过程，并能够达到预期的产品属性。到目前为止，由于巨大的计量要求，许多过程尚未成功实现。所谓的X射线散射是一种适合液相的非破坏性测量技术，非常适合原位过程分析。该提出的项目的目的是开发一种新的超小角度和广角X射线散射设备（USAXS/蜡），以在连续合成过程中对粒子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要使用的光学元件，样品室和检测散射辐射的测量技术来原位对粒子形成过程进行原位分析。与当前的最新状态相比，可以通过使用相应的X射线光学分量来增加样品和检测器之间的距离，从而使最小散射矢量的分辨率提高了约10倍。因此，新测量系统的使用使得可以分析颗粒结构的大小约为400 nm。因此，测得的USAXS散射曲线为在一级粒子水平和聚集水平上阐明结构提供了有用的信息。另外，在广角上同时检测散射曲线可以表征晶体特性。新开发的USAXS/WAXS测量系统旨在通过连续合成二氧化硅多重组和核心壳磁铁矿 - 硅质复合材料来测试。为此，应将适当的微反应器系统连接到测量单元，以便可以通过调整延迟时间来以时间分辨的方式研究粒子合成中的过程。主要目的是通过原位连续监测和控制反应系统中的过程来确保所需的产品质量（粒度分布，骨料特性，壳厚度的分布等）。