4D-STEM crystal orientation and phase mapping is a powerful technique for the nanocharacterisation of materials, as it can provide simultaneous information on phase distributions, grain size, and crystal orientation. However, it can be challenging to separate phases with similar lattice parameters and symmetries (lattice parameter difference of <5%). EDX mapping can be used to separate phases with different chemical compositions but cannot provide crystal orientation information. A combined method leveraging both 4D-STEM and EDX mapping can reduce fitting errors when used between similar phases though this requires synchronisation between scanned electron beam precession, EDX acquisition and a camera for analytical 4D-STEM acquisitions.

In this study, a polycrystalline aluminium foil with added gold nanoparticles was analysed using EDX-assisted 4D-STEM phase analysis. The aluminium and gold exhibit similar lattice constants of 4.049 Å, and 4.078 Å respectively. The integration of scanning, electron beam precession with dedicated fast precession coils, EDX, and Dectris Quadro direct electron detector in the TESCAN TENSOR instrument enabled the collection of high-quality precession diffraction data with rich chemical information. The seamless synchronisation of these components allows for a streamlined and efficient data collection process. To differentiate between aluminium and gold, the chemical information obtained from EDX was utilised to assign weights to the phases in the diffraction pattern matching algorithm, resulting in a more robust phase analysis. By leveraging the chemical information, it was possible to distinguish between phases with similar crystal structures but different compositions, such as aluminium and gold, despite a lattice parameter difference of less than 5%.

Analytical 4D-STEM datasets consisting of simultaneous EDX and precession-assisted 4D-STEM were measured on a TESCAN TENSOR 100 kV STEM, using the Explore user interface for probe and precession alignment, data acquisition, and on-the-fly pattern indexing with kinematical templates. A beam current of 50pA was used with a precession angle of 0.4 degrees. Datasets were collected with and without EDX assistance for phase mapping, their processed orientation and phase maps are shown in Figure 1. The acquisition and processing parameters were otherwise the same for both datasets.

It can be seen from the images in Figure 1, that adding the EDX data to the phase mapping algorithm greatly assisted with the identification of the correct phase, and this can be backed up by observing the distribution of aluminium and gold in the simultaneously acquired EDX map. However, care must be taken to ensure sufficient characteristic X-ray counts from the known phases are present to avoid spurious identification. The orientation data is not significantly changed, as both display the same cubic crystal structure and use the same orientation legend, however, there is a significant change in phase mapping quality and reliability.

Understanding how fluids migrate through rocks and soil is the key to understanding and managing many natural and industrial processes. These processes include rainwater infiltration in soil, migration of oil or other pollutants underground, or storage of hydrogen or CO2 in deep subsurface reservoirs. Fluids migrate through the pore space in rocks or soils, with flow mechanisms governed by the size and shape of the pores, the composition (mineralogy) of the rock or soil, and the properties of the fluids moving through the pore space. A better understanding of the flow processes at the pore scale is essential to comprehension at larger core, or even reservoir scales. Fast dynamic micro-CT imaging at temporal resolutions in the order of seconds makes it possible to capture unsteady-state flow processes, where the pressure and volume of the fluids in the pore space vary over time. Using TESCAN dynamic micro-CT systems, it is possible to analyze these complex dynamic processes inside the pore structure of rocks and soils in the lab.

To visualize the flow of multiple fluids (liquids and/or gasses) in the pore space of a rock, an in-situ device is required. In this case, an X-ray transparent core holder is used: the CH-17MiLR by RS Systems (Norway). The core holder can handle samples of 6 mm diameter up to a length of 30 mm. The maximum working pressure is 100 bar and the maximum temperature is 100 °C for this type of core holder. Samples are placed in a Viton sleeve and up to 4 in-/outlets are present for confining pressure and injection of multiple fluids. The core holder can be fitted on all TESCAN micro-CT systems, enabling in-situ dynamic imaging at pore scale resolution.

In-situ micro-CT, which enables three-dimensional inspection of processes inside a sample under changing external conditions (such as temperature, load, or fluid flow), has mostly been relegated to interrupted processes where the stimulus is paused, also referred to as time-lapse. To enable a more complete picture, TESCAN employs the method of dynamic CT, which is the most advanced subset of time-resolved X-ray imaging. With dynamic CT, the sample is imaged continuously as it is changing under the applied stimulus, without the time gaps inherent in in-situ micro CT.

The difference between dynamic and time-lapse can be thought of as the difference between a smooth video and a stop-motion animation and the associated temporal resolution. The stop motion has clear missing information between events with an effectively poor temporal resolution, while the smooth video provides enough temporal resolution to tell a complete story. Similarly, the advantage of performing continuous acquisition on dynamic micro-CT lies in its ability to perform uninterrupted, true in-situ experiments. This allows the user to continuously capture data throughout the process as well as avoid undesirable relaxation effects which may happen if pausing is required to perform a longer tomographic acquisition.

The examples illustrated here show the capability to acquire fast dynamic micro-CT data in the order of seconds, which allows the user to visualize directly how different fluids move through the pore structure of the rock. They also illustrate a suite of intuitive software tools for dynamic imaging like sliding window reconstruction and flip point detection. These tools allow the user to reduce the huge amount of information that is associated with dynamic scans to relevant moments in time and space or visualize large 4D datasets in easily interpretable 3D volumes. This makes dynamic imaging easy to perform in the lab and greatly reduces the time to result.

Techniques of volume electron microscopy (EM) have become a strong asset in the scientific arsenal when the three-dimensional (3D) ultrastructure of biological samples is to be examined. Serial block-face scanning electron microscopy (SBF-SEM) is one of the prominent volume EM methods and has seen a great increase in implementation across research labs, facilities, and manufacturers [1]. However, there are still bottlenecks in SBF-SEM associated mainly with complex sample preparation protocols and analysis of vast amounts of generated data [2]. Due to numerous complicated steps, it is usually not possible to execute the entire SBF-SEM experiment using tools from a single vendor and the researchers are forced to laboriously assemble their own customized workflows. Another issue is the exchangeability of SBF-SEM systems – some solutions require heavy reconfiguration of the SEM to switch between SBF imaging and standard operation. This makes the microscope a narrowly specialized tool, which is often incompatible with the needs of modern research facilities. Taking these pain points into consideration, we present a lightweight, easy-to-exchange SBF-SEM add-on for TESCAN SEMs, including a dedicated sensitive BSE detector and a software module for volume EM data processing, thus providing tools for the smooth execution of complex SBF-SEM experiments.

With the growing demand for better, safer, more reliable batteries, there is a need for workflows to study batteries in various stages of their development, and at different resolutions. The battery value chain can be seen as a sequence of domains and processes, each with its own imaging and analysis needs. From raw materials to the development of new types of electrodes that are used in single cells, larger modules, or complicated devices, a great amount of research and development is needed to study each step of this value chain.

Although specialized techniques exist to study the materials or devices in each of these sub-domains, linking these analysis techniques together into a single workflow becomes a necessity to fully comprehend the behavior of batteries. Using analytical tools such as micro-computed tomography (micro-CT), and electron microscopy combined with plasma-FIB, TOF-SIMS, and Raman, batteries can be studied from single electrode particles to full cells – even in operando and within their final devices. Correlation between these methods is not trivial, however, since there is a very large variation in the field of view (a few micrometers to several centimeters) and resolution (a few nanometers to several micrometers) of the methods used in this workflow.

The analytical tasks at hand are further complicated by the very reactive behavior of battery electrodes, creating a need for a fully inert transfer environment of samples between different analysis devices. A workflow to do so, including sample preparation under an inert atmosphere, to eliminate contamination of the samples. 

In this work, we show how large-scale analysis using micro-CT is used to study the overall quality of batteries, and how locations requiring further attention are pinpointed for further analysis using electron microscopes. When these locations are found, they are investigated using large-area plasma-FIB cross-sections and tomography. Using the plasma-FIB, large enough areas to study multiple electrode layers in reasonable process times can be exposed. Further analytical tools, such as TOF-SIMS to visualize lithium inside the electrodes, are then used to understand not only the structure but also the chemistry of these batteries.

A Scanning Electron Microscope equipped with a Focused Ion Beam (FIB-SEM) uniquely combined with a compact Time-of-Flight Secondary Ion Mass Spectrometer (ToF-SIMS) [1,2] and a conventional microanalytical method of Energy Dispersive X-Ray Spectrometry (EDS) brings new possibilities in correlated microscopy and spectroscopy [3,4]. Various materials are typically studied by a two-dimensional approach, based on the surface or cross-section analysis. This kind of characterization may be enough to represent basic compositional properties of the analyzed material but for some advanced cases does not provide complete information. For example, if there is an interest in analyzing surface or material inhomogeneity localization in volumetric objects or if a statistical micro and nanostructures evaluation has to be done, volume analysis is preferred. The basic volume analysis in FIB-SEM is based on FIB serial-sectioning and SEM imaging with topographical and material contrast capability. Simultaneous EDS mapping has also become a frequent requirement, providing qualitative information on elemental distribution. However, the information obtainable by EDS is limited to only elements emitting characteristic X-Ray spectra.

In our contribution, we would like to illustrate the information obtainable by adding ToF-SIMS measurement into the serial-sectioning workflow (3D ToF-SIMS) and in combination with EDS (3D EDS), see Figure 1. This approach has been proposed previously, albeit in the context of a dedicated ToF-SIMS instrument with an extra orthogonal FIB column [5]. ToF-SIMS signal is, unlike EDS, affected

by types of chemical bonds within the material, and it can easily map the distribution of Li and Li-based molecules. Therefore the ToF-SIMS has proved to be a powerful stand-alone or complementary technique to EDS, especially in battery research. The ToF-SIMS analysis combined with the FIB-slicing minimizes the effect of locally uneven milling rate on chemically and structurally heterogeneous samples, leading to severe deformation of the dataset as the sputtering progress in some areas faster than in others as a typical property of standard ToF-SIMS analysis.

Using the above-described method, we illustrate, on an inertly transferred Li battery component, all the possible information that can be gathered to aid in the understanding of the inner properties, from porosity, particles damage, delamination, chemical contamination, and results of parasitical chemical reactions. This overview information allows for example evaluation of battery material degradation and its root causes, such as mechanical damage, Li dendrite growth, or chemical contamination. The limitations of this method will also be discussed, from geometrical sample requirements to relations between minimal slice thickness and ion dose applied during the ToF-SIMS measurements.

The standard procedure for preparing cross sections using the FIB-SEM technique is to use high currents to remove material quickly, then reduce the FIB current to obtain better beam profile and consequently, a better quality for the final surface. Reducing the maximum current used for final polishing of the section surface, however, results in a longer preparation process. For small cross sections with sizes in the tens of μm, this current reduction method is acceptable. However, as the size of the cross-sectional area to be polished increases, the analysis time increases substantially; therefore, this method is not suitable for preparing cross sections with sizes in the hundreds of μm. To overcome this limitation for large cross sections, plasma FIB was introduced to deliver higher beam currents than those achievable with conventional Ga FIB-SEMs. Plasma FIB-SEM provides several advantages for sample characterization. First, its high current ion beam is capable of high material sputtering rates which enables efficient preparation of large trenches or cross sections.

Plasma FIB also can be used for polishing large surface areas, thereby enhancing sample
features and providing more detailed contextual information about structure and composition. about the sample. This can help to reveal material distribution, obtain better statistical information, and link the microscale to the nanoscale sample characterization. Several technologies have been introduced that improve the implementation of high current plasma FIB for large scale materials characterization. In this webinar, we will walk through the typical plasma FIB cross-sectioning workflow and discuss high current polishing methods. We will present TESCAN’s TRUE X-Sectioning TESCAN Rocking Stage, which were developed to suppress artifacts and improve the final cross section surface quality when using high beam currents for final polishing.

Finally, we will show how plasma FIB-SEM speeds not only cross section preparation, but also enables a greater understanding of your materials by improving 3D FIB-SEM tomography analyses

The powder bed fusion-laser beam method is utilized in additive manufacturing to process novel
materials. This method has been employed for preparing aluminum-based materials, allowing for control over their microstructure and resulting properties. This poster focuses on two variants from the Al-Mn- Cr-Zr alloy family, which were prepared using the plasma FIB-SEM technique. By employing in-situ synchrotron scanning X-ray fluorescence, we investigate the distribution of Mn, Cr, and Fe, thereby demonstrating the nucleation and growth of different precipitates in the material at elevated temperatures. These developed precipitates contribute significantly to the hardness enhancement observed during annealing after printing. Therefore, comprehending the behaviour of materials and the formation of precipitates at higher temperatures is a vital step in both basic and applied research for material development.

Successful synchrotron experiments rely on meticulous sample preparation. Conventional Ga FIB-SEM techniques often result in Ga segregation to the grain boundaries in Al alloys, leading to challenges/ To overcome this issue, we employed plasma FIB-SEM, utilizing inert Xe+ ions to prevent chemical interference with microstructural evolution at grain orientation and type were confirmed using EBSD and EDS techniques. Precise navigation during individual sample preparation was achieved using SEM
contrast. Cubic specimens with dimensions of 10 μm x 30 μm and 50 μm x 50 μm and a thickness of 1 μm were prepared using FIB and selected from specific areas of interest. The preparation process
involved multiple steps, including transferring the samples to chips for subsequent in-situ heating
experiments conducted at the synchrotron.

Many dynamic interactions within the cell microenvironment modulate cell behavior and cell fate. However, the pathways and mechanisms behind cell–cell or cell–extracellular matrix interactions remain understudied, as they occur at a nanoscale level.

Recent progress in nanotechnology allows for mimicking of the microenvironment at nanoscale in vitro; electron-beam lithography (EBL) is currently the most promising technique. Although this nanopatterning technique can generate
nanostructures of good quality and resolution, it has resulted, thus far, in the production of only simple shapes (e.g., rectangles) over a relatively small area (100 × 100 μm), leaving its potential in biological applications unfulfilled.

Here, we used EBL for cell-interaction studies by coating cell-culture-relevant material with electron-conductive indium tin oxide, which formed nanopatterns of complex nanohexagonal structures over a large area (500 × 500 μm). We
confirmed the potential of EBL for use in cell-interaction studies by analyzing specific cell responses toward differentially distributed nanohexagons spaced at 1000, 500, and 250 nm.

We found that our optimized technique of EBL with HaloTags enabled the investigation of broad changes to a cell-culture-relevant surface and can provide an understanding of cellular signaling mechanisms at a single-molecule level.

Printed circuit boards (PCBs) are at the heart of numerous advancements in electronic science and technology, and as such they are expected to work flawlessly and as designed. Errors, no matter how seemingly minor, cannot be tolerated because PCBs are used in many highly technological applications, such as those supporting aerospace, biotechnology, automotive, military, and many more industries. There exist many PCB testing protocols, such as in-circuit testing or bare board testing; however, these tests may not detect performance issues that are outside of their testing ranges. So, these PCBs are most often subject to additional optical and internal validation. One technique for visualizing inside PCB materials is X-ray imaging, which can be used to build an understanding of the material’s internal structure and any possible defects. Examples of defects that may occur are micro-cracks, component misalignment, voids, and an excess of solder.

As PCBs become more densely populated, with hundreds of smaller components and multiple layers of material mixes, a single radiography approach has limitations. In this study, we will highlight the use of the full X-ray energy spectrum by using spectral radiography to discern the individual materials present. With this approach, components in a mixed or multi-layered electronic device become visible.

Conventional and spectral X-ray imaging is, of course, not limited to the analysis of PCBs. As an example, a multi-modal conventional and spectral CT study was performed on a smart ring wearable electronic device. Wearable electronic devices are becoming increasingly popular and are packed with different sensors to measure temperature, heart rate, blood oxygen, or movement. In addition, these devices need components such as batteries, antennas, or gyroscopes to monitor and transmit data about the person wearing them. Given the unconventional shape of some of these components, it is crucial to assess and understand the internal connections once they are fitted into the final device.

The combination of conventional CT and radiography with their spectral counterparts is a powerful way to gain insights into electronic components. Where CT can be seen as the gold standard for non-destructive 3D characterization, spectral CT makes it possible to actually identify gold. By harnessing the multi-energy information from a single spectral radiography acquisition, it is possible to discern within a radiograph the presence of different materials in the X-ray path. An unlimited number of materials can be distinguished from the full spectral information, even without pre-tuning the acquisition parameters as is often required in classical dual-energy approaches. The spectral information allows us to select regions of interest that are eligible to further investigation with high-resolution CT imaging closing the failure analysis track and eventually leading to failure-free devices.