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Article Magnetic Compton Scattering Study of Li-Rich Battery Materials Kosuke Suzuki 1,∗ , Yuji Otsuka 1, Kazushi Hoshi 1, Hiroshi Sakurai 1 , Naruki Tsuji 2 , Kentaro Yamamoto 3 , Naoaki Yabuuchi 4 , Hasnain Hafiz 5 , Yuki Orikasa 6 , Yoshiharu Uchimoto 3 , Yoshiharu Sakurai 2 , Venkatasubramanian Viswanathan 5 , Arun Bansil 7 and Bernardo Barbiellini 7,8 Citation: Suzuki, K.; Otsuka, Y.; Hoshi, K.; Sakurai, H.; Tsuji, N.; Yamamoto, K.; Yabuuchi, N.; Hafiz, H.; Orikasa, Y.; Uchimoto, Y.; et al. Magnetic Compton Scattering Study of Li-Rich Battery Materials. Condens. Matter2022,7,4. https://doi.org/ 10.3390/condmat7010004 Academic Editor: Bohayra Mortazavi Received: 11 November 2021 Accepted: 24 December 2021 Published: 28 December 2021 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). 1 2 3 4 5 6 7 Abstract: The redox process in a lithium-ion battery occurs when a conduction electron from the lithium anode is transferred to the redox orbital of the cathode. Understanding the nature of orbitals involved in anionic as well as cationic redox reactions is important for improving the capacity and energy density of Li-ion batteries. In this connection, we have obtained magnetic Compton profiles (MCPs) from the Li-rich cation-disordered rock-salt compound LixTi0.4Mn0.4O2 (LTMO). The MCPs, which involved the scattering of circularly polarized hard X-rays, are given by the momentum density of all the unpaired spins in the material. The net magnetic moment in the ground state can be extracted from the area under the MCP, along with a SQUID measurement. Our analysis gives insight into the role of Mn 3d magnetic electrons and O 2p holes in the magnetic redox properties of LTMO. Keywords: Li-rich cathode material; magnetic property; magnetic Compton profile 1. Introduction Lithium-rich disordered cathode materials, such as LixTi0.4Mn0.4O2 (LTMO), are at- tracting a lot of current attention because their capacity can reach 300 mAhg−1 [1], which is significantly greater than that of the conventional cathode materials. For example, LiCoO2 has a capacity of 140 mAhg−1, and LiFePO4 has a capacity of 170 mAhg−1. Although the high capacity of the Li-rich cathode materials has been suggested to result from a combina- tion of cationic and anionic redox processes [2], a fundamental understanding of the redox mechanism at play in Li-rich cathode materials is needed for optimizing their performance. Details of the anionic redox mechanisms are not fully understood because experiments that can directly probe redox orbitals are limited. In this connection, Hafiz et al. have reconstructed the orphaned O− 2p orbital of LTMO in momentum space by combining high-energy X-ray Compton scattering with accurate first-principles calculations [3]. This visualization was enabled by the bulk sensitivity of the Compton scattering technique. Studies of redox orbitals in other cathodes materials include LiCoO2 [4], LiMn2O4 [5,6], and LiFePO4 [7]. Moreover, the imaging Compton technique has been applied to in operando and in situ measurements to monitor the lithiation state of commercial batter- ies, see Ref. [8] and references therein. There are fundamental difficulties in visualizing redox orbitals using X-ray photoemission spectroscopy (XPS) [9], soft X-ray absorption Graduate School of Science and Technology, Gunma University, Kiryu 376-8515, Japan; t201d016@gunma-u.ac.jp (Y.O.); hoshi@gunma-u.ac.jp (K.H.); sakuraih@gunma-u.ac.jp (H.S.) Japan Synchrotron Radiation Research Institute (JASRI), Sayo 679-5198, Japan; ntsuji@spring8.or.jp (N.T.); sakurai@spring8.or.jp (Y.S.) Graduate School of Human and Environmental Studies, Kyoto University, Kyoto 606-8501, Japan; yamamoto.kentaro.4e@kyoto-u.ac.jp (K.Y.); uchimoto.yoshiharu.2n@kyoto-u.ac.jp (Y.U.) Department of Chemistry and Life Science, Yokohama National University, Yokohama 240-8501, Japan; yabuuchi-naoaki-pw@ynu.ac.jp Department of Mechanical Engineering, Carnegie Mellon University, Pittsburgh, PA 15213, USA; hafiz.h@northeastern.edu (H.H.); venkatv@andrew.cmu.edu (V.V.) Department of Applied Chemistry, Ritsumeikan University, Kusatsu 525-8577 Japan; orikasa@fc.ritsumei.ac.jp Department of Physics, Northeastern University, Boston, MA 02115, USA; ar.bansil@northeastern.edu (A.B.); Bernardo.Barbiellini@lut.fi (B.B.) Department of Physics, School of Engineering Science, LUT University, 53850 Lappeenranta, Finland 8 * Correspondence: kosuzuki@gunma-u.ac.jp; Tel.: +81-277-30-1714 Condens. Matter 2022, 7, 4. https://doi.org/10.3390/condmat7010004 https://www.mdpi.com/journal/condensedmatterPDF Image | Magnetic Compton Scattering Study of Li-Rich Battery Materials
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