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While advances have been made using SC\u2010NCM cathode materials, careful studies of cathode degradation mechanisms are scarce. Herein, we employed quasi single\u2010crystalline LiNi<jats:sub>0.65<\/jats:sub>Co<jats:sub>0.15<\/jats:sub>Mn<jats:sub>0.20<\/jats:sub>O<jats:sub>2<\/jats:sub> (SC\u2010NCM65) to test the relationship between cycling performance and material degradation for different charge cutoff potentials. The Li\/SC\u2010NCM65 cells showed &gt;77\u2009% capacity retention below 4.6\u2005V vs. Li<jats:sup>+<\/jats:sup>\/Li after 400 cycles and revealed a significant decay to 56\u2009% for 4.7\u2005V cutoff. We demonstrate that the SC\u2010NCM65 degradation is due to accumulation of rock\u2010salt (NiO) species at the particle surface rather than intragranular cracking or side reactions with the electrolyte. The NiO\u2010type layer formation is also responsible for the strongly increased impedance and transition\u2010metal dissolution. Notably, the capacity loss is found to have a linear relationship with the thickness of the rock\u2010salt surface layer. Density functional theory and COMSOL Multiphysics modeling analysis further indicate that the charge\u2010transfer kinetics is decisive, as the lower lithium diffusivity of the NiO phase hinders charge transport from the surface to the bulk.<\/jats:p>","DOI":"10.1002\/anie.202305281","type":"journal-article","created":{"date-parts":[[2023,6,7]],"date-time":"2023-06-07T13:27:17Z","timestamp":1686144437000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":26,"title":["Quantifying Degradation Parameters of Single\u2010Crystalline Ni\u2010Rich Cathodes in Lithium\u2010Ion Batteries"],"prefix":"10.1002","volume":"62","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0868-8404","authenticated-orcid":false,"given":"Wengao","family":"Zhao","sequence":"first","affiliation":[{"name":"Institute of Nanotechnology Karlsruhe Institute of Technology (KIT)  Hermann-von-Helmholtz-Platz\u20051 76344 Eggenstein-Leopoldshafen 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