---

Advanced Real Time Imaging: Emerging Imaging Techniques
Sponsored by: TMS Functional Materials Division, TMS Structural Materials Division, TMS: Advanced Characterization, Testing, and Simulation Committee, TMS: Alloy Phases Committee, TMS: Biomaterials Committee
Program Organizers: Jinichiro Nakano, MatterGreen; David Alman, National Energy Technology Laboratory; Il Sohn, Yonsei University; Hiroyuki Shibata, Tohoku University; Antoine Allanore, Massachusetts Institute of Technology; Noritaka Saito, Kyushu University; Zuotai Zhang, Southern University of Science and Technology; Bryan Webler, Carnegie Mellon University; Wangzhong Mu, KTH Royal Institute of Technology; Pranjal Nautiyal, Oklahoma State University; Jiawei Mi, University of Hull

Tuesday 8:00 AM
March 5, 2024
Room: Blue Spring II
Location: Hyatt

Session Chair: Jinichiro Nakano, MatterGreen; Jiawei Mi, University of Hull

---

8:00 AM  Invited
Real-time and In-situ Measurements Using High-speed AFM: Stacy Moore¹; Tomas Martin¹; Oliver Payton²; Loren Picco²; ¹University of Bristol; ²Bristol Nano Dynamics Ltd.
     Contact-mode high-speed atomic force microscopy (HS-AFM) is capable of collecting topographic maps of a sample surface with nanometre-scale lateral, atomic-scale height, and sub-second temporal resolutions. The rapid throughput of HS-AFM enables high-resolution imaging across large areas of a sample surface for feature distribution analysis and correlative analysis using techniques such as scanning electron microscopy. Such measurements can be performed in ambient conditions or in liquid environments for in-situ, in-operando, in-vitro, and in-vivo experiments. Additional functionalities include parallel potentiostatic control and thermal or electrical conductivity mapping.The presented work explores the wide range of applications for HS-AFM in materials and corrosion science including stress corrosion cracking (SCC), electrodeposition, and large area precipitation analysis. For the study of localised corrosion processes such as SCC or pitting corrosion, the high temporal resolution of this instrument allows unequivocal understanding of the nanoscale mechanisms and the order by which they occur through direct observation.

8:40 AM  Invited
Picosecond Laser Ultrasound Spatial and Temporal Tracking of Material Property Changes Under Irradiation: Elena Botica Artalejo¹; Greg Wallace¹; Eleni Mowery¹; Myles Stapelberg¹; Aljazzy Alahmadi¹; Saleem Al Dajani¹; Benjamin Dacus¹; Jonas Rajagopal¹; Angus Wylie¹; Michael Short¹; ¹Massachusetts Institute of Technology
    Higher dimension experiments have the promise to hasten many fields in materials science, particularly those involving irradiation due to their inherent cost, danger, and difficulty. Optimizing a material’s property response to irradiation, or even simply studying it, too often requires either huge experimental efforts or sparse matrices of experimental parameters. In this talk, we review emerging ways in which picosecond ultrasonic inference of material properties of interest can reduce the dimensionality of irradiation materials experiments. Examples ranging from in situ deduction of radiation response kinetics for structural material lifetime studies, to quickly searching ternary and higher-order compositional systems for radiation robustness, to helping determine which defects may be responsible for recently observed, irradiation-enhanced superconductivity. The common links between these studies are the use of picosecond ultrasound to infer properties or defects of interest, as well as orders of magnitude faster experimentation when using these inference models.

9:00 AM  
Limited Angle X-ray Nanotomography Captures Solidification in 4D: Soumyadeep Dasgupta¹; Kyle Farmer¹; Paul Chao¹; Shanmukha Kiran Aramanda¹; Xianghui Xiao²; Elizabeth Holm¹; Ashwin Shahani¹; ¹University of Michigan; ²Brookhaven National Laboratory
    By studying solidification in real-time, we gain direct insight on the interfacial dynamics, leading to improved control, design, and development of technological materials. In particular, synchrotron x-ray nanotomography offers a 3D view of microstructural evolution at the nanoscale. Unfortunately, the temporal resolution is limited by the hardware capabilities of the microscope. To improve the temporal resolution to the sub-minute regime, we employ Limited Angle Tomography (LAT). We investigate via LAT the directional solidification of a near-eutectic Al-Al₃Ni alloy as a proof-of-concept. A novel image processing and composite reconstruction approach allow us to mitigate artifacts generated by LAT and visualize the eutectic solidification process in 3D space and time. This technique offers promise not only in solidification science but also in 3D characterization of other phenomena which require higher temporal resolution within a limited viewing window.

9:20 AM  
Probing the Dynamics of Materials with Ultrafast Transmission Electron Microscopy: Volkan Ortalan¹; ¹University of Connecticut
    Latest advances in instrumentation have made it a very exciting time to perform both fundamental and applied research in the electron microscope. In situ microscopy is moving forward at a rapid pace with the development of gas/liquid stages that permit reaction processes to be imaged and analyzed at atomic resolution. Furthermore, the development of nanosecond and faster photoemission electron sources offers the chance to move the high spatial resolution world of electron microscopy into the ultrafast world of materials dynamics. The combination of these capabilities allows for vast improvements of in situ TEM studies limited by video rate in that many processes span multiple time and length scales. In this presentation, examples of ultrafast transmission electron microscopy studies will be presented for selected materials systems. Short lived transient processes involved in dynamic processes in materials will be discussed to obtain new insights.

9:40 AM Break

10:00 AM  Invited
Depicting Fast Processes in Real-time by Ultra-high Speed Synchrotron-based Hard X-ray Imaging: Alexander Rack¹; ¹European Synchrotron Radiation Facility
    The potential of hard X-ray imaging to tackle scientific questions especially related to materials sciences can be substantially increased when the dimension time is accessible. Nowadays, unprecedented temporal resolution with hard X-ray imaging can be reached at synchrotron light sources thanks to high-speed CMOS cameras combined with indirect detection schemes and polychromatic illumination. The success of real-time X-ray imaging is underlined by numerous scientific studies: bending and welding of stainless steel require high photon energies above 100 keV but moderate acquisition rates of a few 1000 images/s. Studies of thermal abuse testing of Li-ion batteries are similar but on top need sophisticated safety installations. Visualization of laser-processing of metals is more demanding in speed (up to several 100 000 images/s). Ultimately, processes such as shock-induced cavity collapse require acquisition rates up to the MHz regime. In this presentation, we shall outline the established capabilities at synchrotron light sources.

10:20 AM  Invited
Towards MHz X-ray High-resolution Holography at European XFEL: Patrik Vagovic¹; Tokushi Sato²; Jayanath Koliyadu²; Sarlota Birnsteinova²; Johan Bielecki²; Trey Guest²; Marcin Sikorski²; Marco Ramilli²; Richard Bean²; Romain Letrun²; Rita Graceffa²; Antonio Bonucci²; Luigi Adriano²; Abhisakh Sarma²; Peter Szeles³; Daniel Moško³; Kristián Sabol³; Pablo Villanueva Perez⁴; Jozef Uličný³; ⁴; Alke Meents¹; Henry Chapman¹; ¹CFEL, DESY; ²European XFEL; ³Šafárik University; ⁴Lund University
    To enable the study of stochastic phenomena in micrometer scales, with objects and features propagating with velocities reaching km/s we have recently demonstrated implemented MHz X-ray imaging capability at EuXFEL. Such high-speed sampled X-ray microscopy enables to study of stochastic phenomena by recording sharp X-ray images with ~20fs exposure of each frame separated by 886ns or smaller. MHz X-ray microscopy was recently applied to study the exfoliation of graphite under an ultrasound wave field in water as a first-user experiment enhancing method pool at EuXFEL for a broader user community. As further development step, MHz X-ray multi-projection X-ray imaging is being implemented via EIC Pathfinder project, with recent proof of principle experiment at SPB/SFX instrument. We will present recent developments which will enable MHz X-ray holography with spatial resolution down to 0.3 micrometers with high dynamic range providing enough sensitivity for resolving small density variations in stochastic systems.

10:40 AM  
XRF: A New Materials-science Research Facility for the International Space Station: Wilhelmus Sillekens¹; Guillaume Reinhart²; Ana Frutos Pastor¹; Antonella Sgambati¹; ¹European Space Agency; ²Aix-Marseille Univ, Université de Toulon
    Materials research in space is a niche within the materials science and engineering domain. Still, scientists have been pursuing such research for decades now using platforms as sounding rockets, Spacelab and the International Space Station (ISS) to exclude gravitationally driven effects like buoyancy/sedimentation and convective flow in for instance solidification processes. The European Space Agency is currently developing a facility for the ISS which is to enable in-situ and time-resolved observation of metal-alloy solidification using X-ray radiography, amongst others. This X-Ray Facility (XRF) will consist of a core unit (with a microfocus X-ray source) and an experiment unit including diagnostics (e.g., a furnace with crucible/sample and scintillator/camera), enabling the real-time imaging of the process. The report will introduce the background and heritage, its features and specifications, as well as the development status of and preliminary and prospective investigations with this facility, which is to become operational on orbit by 2026.

---