ZEISS at Microscopy & Microanalysis (M&M) 2023

Extending FIB-SEM by fs-laser integration to address materials challenges for R&D, quality control and FA

Exploring the Power of Serial Block-Face Imaging: A Key Technology in the Volume EM Revolution

X-ray Microscopy: Bringing Multiscale 3D Volume Imaging to Plant Biology

The Role of Correlative CT and EM Investigations in the Development of Li ion Battery Technology

The increasing miniaturization and individualization of advanced materials and components, coupled with higher material purity and manufacturing quality, have made identifying and investigating failures more challenging yet critical in R&D as well as quality control and failure analysis. Precisely locating and preparing target areas deeply buried and sparsely distributed necessitates advanced techniques. While standard materialographic approaches combined with CT scans are commonly used, their targeting precision relies heavily on machine capabilities and the skill of the user. An alternative method involves correlative approaches that combine CT or X-Ray Microscopy with high-precision FIB preparation. Although this achieves high accuracy, the limited width and depth of FIB restrict it to near-surface features. To overcome these issues, an integrated system combining a femtosecond (fs-) laser with a standard FIB/SEM was introduced. The integrated system enables seamless transitions between various preparation modes, saving time and effort compared to using separate systems that require sample transfer and extensive alignment. The addition of a fs-laser widens the application space for sample preparation and manipulation from only 100 µm to the mm range. By the example of different advanced materials samples and components the talk will outline the benefits of utilizing an integrated system with regard to accuracy, time savings and knowledge generation in both R&D and quality control / failure analysis environments.

Imaging in plant biology is a critical aspect of understanding growth and development, particularly for meristems and inflorescence structures. In addition, understanding the interaction of roots with soil is crucial, but it is difficult as these processes occur underground. Capturing detailed 3D image data of these delicate structures and complicated environments is difficult for conventional microscopy. X-ray microscopy (XRM) bridges this imaging gap by providing multiscale high-resolution 3D tomographic data where cell-level volumes can be situated within the context of the whole structure. XRM is a powerful tool for visualizing root-soil-microbe interactions in situ without having to dig up the root system. Correlative imaging is also significantly enhanced by using XRM of whole resin-embedded plant samples as a road map for nanometer-scale volume electron microscopy, avoiding the uncertainty of sectioning blindly through a sample. Use of XRM in the multiscale and multimodal analysis of 3D plant features using economically and scientifically important plant systems will be presented.

Batteries and related energy storage systems are one of the dominant factors in the global transition to renewable energy use. Here we report on investigations aiming at a scale-bridging and three-dimensional understanding of Li-ion battery electrodes and their functionalities. Therefore, we employ microCT and nanoCT investigations, which provide very valuable insight in battery structures and ageing mechanisms, in a complementary way to gain three-dimensional information on multiple length scales. In a correlative approach, these investigations are then combined with higher resolution electron microscopy characterization of the electrode microstructures, the anode and cathode materials and the surfaces and interfaces of a broad range of battery materials. The scale bridging results on materials and functionalities can be employed to design novel battery materials with improved storage capacities and to optimize the properties of the resulting concepts.

At the core of our activities, MicroCT and NanoCT were used to determine the three-dimensional microstructure of the electrode samples. The MicroCT images were collected on a ZEISS Xradia 520 Versa 3D X-ray Microscope, and NanoCT was performed on a ZEISS Xradia 810 Ultra 3D X-ray Microscope. The increased resolution of the 810 Ultra provides a very detailed picture of the active material, with microstructural details clearly resolved. Because of the lower x-ray energy used in the 810 Ultra, however, the sample geometries have to be limited to several tens of micrometers in diameter. The CT images of the new and the aged cell can be visually and analytically compared and offer valuable insights in the structural changes during the ageing process. Future activities will include novel approaches for correlative data management and AI-based analysis of the combined CT and EM results.