Development of multidimensional analysis of particulate systems using analytical centrifugation

复杂粒子系统的性质取决于其大小、形状和组成，其合成和应用越来越受到科学技术的关注。因此，颗粒表征起着核心作用，而动态光散射（DLS）和电子显微镜等已建立的方法要么缺乏分辨率和准确性，要么费力费时。因此，本项目的目的是建立分析离心（AC）作为颗粒技术领域中具有高精度和无与伦比的分辨率的标准测量程序。与上述已建立的表征方法相比，AC具有一些明显的优势，例如绝对测量原理和同时表征多达12个样品的可能性。该项目的重点是颗粒特性的多维表征，例如尺寸和形状或尺寸和密度，颗粒尺寸从10 nm到100 µm。为了实现这一目标，不仅需要新的测量和评估方法，而且需要改进现有的AC设置。工业合作伙伴LUM GmbH将通过开发新的交流转子设置来改善测量过程中的温度控制。因此，温度不稳定性的影响被最小化，并且测量精度将明显提高。此外，LUM GmbH将开发和优化二维颗粒分析所需的扇形比色皿。同时，将在申请人的研究所对AC涵盖的粒度、密度和浓度的测量范围进行评价。由于测量范围明确，用户可以估计AC是否适合表征特定样品。之后，扇形比色皿将用于同时测定两种颗粒性质，即粒度和形状以及粒度和密度。此外，在分析超离心（AUC）领域中已知的用于二维颗粒分析的测量技术和评估协议将被转移到AC并仔细建立。因此，通过该项目，AUC多维颗粒分析的完整能力可用于AC。通过将所有开发的方法应用到LUM GmbH的现有软件中，将为科学和技术领域的广泛用户提供高分辨率的综合沉降分析方法。

The synthesis and application of complex particle systems, whose properties depend on their size, shape and composition, is getting more and more in the focus of science and technology. Therefore, particle characterization plays a central role, whereas established methods like dynamic light scattering (DLS) and electron microscopy either have a lack in resolution as well as accuracy or are laborious and time-consuming. Accordingly, aim of the present project is the establishment of analytical centrifugation (AC) as a standard measurement routine with high accuracy and unrivaled resolution in the field of particle technology. AC has some clear advantages over the aforementioned established characterization methods, for instance the absolute measurement principle and the possibility for the simultaneous characterization of up to twelve samples. The focus of this project is the multidimensional characterization of particle properties, e.g. size and shape or size and density, for particle sizes from 10 nm up to 100 µm. To achieve this goal, not only new measurement and evaluation methods but also improvements of the present AC setup are required. By developing a new rotor setup for AC, the industrial partner LUM GmbH will improve the temperature control during the measurements. Thus, the influence of temperature instabilities is minimized and the measurement accuracy will be clearly enhanced. Furthermore, LUM GmbH will develop and optimize sector shaped cuvettes that are required for two-dimensional particle analysis. Meanwhile, the evaluation of the measurement range in terms of particle size, density and concentration covered by AC will be performed at the institute of the applicant. Due to the well-defined measurement range, the user can estimate whether AC is appropriate for characterizing the specific sample. Afterwards the sector shaped cuvettes will be used for the simultaneous determination of two particle properties, i.e. particle size and shape as well as particle size and density. In addition, measurement techniques and evaluation protocols for the two-dimensional particle analysis which are already known in the field of analytical ultracentrifugation (AUC) will be transferred to AC and carefully established. Thus, by means of this project the complete capability of AUC for multidimensional particle analysis gets accessible for AC. By implementing all developed methods into the existing software of LUM GmbH, comprehensive methods of sedimentation analysis with high resolution will be available for a wide range of users from science and technology.