How can nanoscale chemical transformations be characterized by X-ray spectromicroscopy?
David A. Shapiro, Jiangtao Zhao, and their colleagues at Berkeley Lab, aBeam Technologies Inc., Argonne National Laboratory, and Universiy of California – Berkeley, and the University of Science and Technology of China published on their use of the Hummingbird Scientific in-situ liquid flow X-ray sample holder to characterize chemical transformations in LixFePO4 battery cathode platelets using in-situ heating and ultrahigh-resolution soft X-ray microscopy.
Conventional (a) and (b) and ptychographic (c) and (d) spectromicroscopy of LixFePO4 microplatelets. Point spectra from conventional scanning (dashed lines) and ptychographic modes (dotted lines with circles) are shown in (e). Reference spectra from pure materials are also shown for comparison. f-g) Heating experiment showing the redistribution of chemical components when the sample is heated from f) room temperature to g) 300°C. Copyright © 2020 American Association for the Advancement of Science. All rights reserved
X-ray ptychography and conventional scanning X-ray microscopy are both employed to characterize a transformation from LiFePO4 to FePO4 that occurs upon heating from room temperature to 300 °C. Ptychographic mode proved useful for visualization of the smallest nanoscale features. The liquid cell environment protected the sensitive particles from air exposure as well as electron beam damage. The work demonstrated this powerful approach to operando characterization of chemical and structural changes to heterogeneous nanomaterials using the in-situ liquid flow X-ray sample holder.
Reference: David A. Shapiro, Sergey Babin, Richard S. Celestre, Weilun Chao, Raymond P. Conley, Peter Denes, Bjoern Enders, Pablo Enfedaque, Susan James, John M. Joseph, Harinarayan Krishnan, Stefano Marchesini, Krishna Muriki, Kasra Nowrouzi, Sharon R. Oh, Howard Padmore, Tony Warwick, Lee Yang, Valeriy V. Yashchuk, Young-Sang Yu, and Jiangtao Zhao, Science Advances 6 (51) (2020) DOI: 10.1126/sciadv.abc4904
Full paper Copyright © 2020 American Association for the Advancement of Science. All rights reserved.
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