DOE OSTI · 2561429
In Situ Diffraction and Ex Situ Transmission X‐Ray Microscopy Studies of Solid‐State Upcycling for NMC Cathodes
Abstract
Upcycling of recycled LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) cathodes offers an economical route to produce cathode materials with increased energy density (i.e., LiNi 0.8 Mn 0.1 Co 0.1 O 2 , NMC811) that meet the performance needs of present-day electric vehicles. In this work, solid-state upcycling of NMC622 via calcination with Ni(OH) 2 and LiOH was monitored using in situ synchrotron powder X-ray diffraction measurements. Sequential Rietveld refinements indicate that the calcination proceeds by initially converting Ni(OH) 2 to a rocksalt NiO phase followed by lithiation of NiO to form LiNiO 2 (LNO), with both NMC and LNO phases present in nearly equal proportions at the calcination endpoint. Variable-energy transmission X-ray microscopy tomograms of upcycled samples reveal that the NMC and LNO domains are intermixed at sub-micron length scales. Depth-dependent analysis of multi-elemental fitting maps matches the expected NMC811 composition at the secondary particle level and indicates that transition metal diffusion is not limited by the secondary particle size.
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Nisbet, Matthew L. [Argonne National Laboratory (ANL), Argonne, IL (United States)] (ORCID:0000000195319193), Luong, Diana [Argonne National Laboratory (ANL), Argonne, IL (United States)] (ORCID:000000024093687X), Allen, Eva Michelle [Argonne National Laboratory (ANL), Argonne, IL (United States)] (ORCID:0000000348506492), Park, Sohyun [Argonne National Laboratory (ANL), Argonne, IL (United States)], Kinnibrugh, Tiffany L. [Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)] (ORCID:0000000218981869), Stubbs, Joanne E. [Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)] (ORCID:0000000285092009), Eng, Peter J. [Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)] (ORCID:0000000280723203), Vaughey, John T. [Argonne National Laboratory (ANL), Argonne, IL (United States)] (ORCID:0000000225566129), Fister, Tim T. [Argonne National Laboratory (ANL), Argonne, IL (United States)] (ORCID:0000000165376170). 2025-04-21. In Situ Diffraction and Ex Situ Transmission X‐Ray Microscopy Studies of Solid‐State Upcycling for NMC Cathodes. https://doi.org/10.1002/aenm.202500698
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