Fast in situ 3D characterization of nano-materials with X-ray full-field nano-tomography: latest developments at the Advanced Photon Source

V. De Andrade, M. Wojcik, A. Deriy, S. Bean, D. Shu, P. KC, F. De Carlo
Argonne National Laboratory,
United States

Keywords: nanotomography, TXM, materials science, X-ray


The Transmission X-ray Microscope (TXM) at beamline 32-ID of the Advanced Photon Source beamline at Argonne National Laboratory has been tailored for high throughput and high spatial resolution in operando nano-tomography experiments [1]. Thanks to a constant R&D effort during the last five years of operations, it emerged as a highly scientific productive instrument, especially in the domain of Materials Science and a leader in term of spatial resolution with sub 20 nm resolving power in 3D, with full dataset collection speed that can be as short as 1 min. The TXM benefits from the in-house development of cutting-edge X-ray optics, complex opto-mechanical components and a suite of software including TomoPy, an open-sourced Python toolbox to perform tomographic data processing and image reconstruction, and others based on machine learning to push the limit of 3D nano-imaging while reducing the total X-ray dose. It operates either with a fast moderate spatial resolution (40 - 50 nm) mode with a large field of view of ~50 μm or with a very high spatial resolution of 16 nm and a smaller field of view of ~10 μm. This presentation will give an overview of experiments covering many scientific fields like ex and in situ battery characterization [2-4], dynamic experiments with one-minute temporal resolution on cement formation, crystal growth / dissolution phenomena [5], neuroscience [6], etc. In addition, a new projection microscope currently under development at 32-ID and expected to be operational by September 2019 will be introduced. This new instrument will provide high-speed full-field nano-tomography targeting 20 nm spatial resolution and will operate in phase contrast mode (holography). With a high coherent synchrotron source, this technique is proven very efficient for characterizing low-Z materials like Li oxide, black carbon or polymers. A comparison of such materials characterization with TXM and Projection Microscopy will be shown. References [1] De Andrade, Vincent, et al. "Nanoscale 3d imaging at the advanced photon source." SPIE Newsroom (2016): 2-4. [2] S. Müller, P. Pietsch, B. E. Brandt, P. Baade, V. De Andrade, F. De Carlo & V. Wood. "Quantification and modeling of mechanical degradation in lithium-ion batteries based on nanoscale imaging." Nature Communication, volume 9, Article number: 2340 (2018). [3] Zhao, Chonghang, et al. "Imaging of 3D morphological evolution of nanoporous silicon anode in lithium ion battery by X-ray nano-tomography." Nano energy 52 (2018): 381-390. [4] Lim, Cheolwoong, et al. "Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries." Journal of synchrotron radiation 24.3 (2017): 695-698. [5] Yuan, Ke, et al. "Pb2+–Calcite Interactions under Far-from-Equilibrium Conditions: Formation of Micropyramids and Pseudomorphic Growth of Cerussite." The Journal of Physical Chemistry C 122.4 (2018): 2238-2247. [6] Yang, Xiaogang, et al. "Low-dose x-ray tomography through a deep convolutional neural network." Scientific reports 8.1 (2018): 2575.