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Precise control of the calcination chemistry is therefore crucial for synthesizing state\u2010of\u2010the\u2010art Ni\u2010rich layered oxides (LiNi<jats:sub>1\u2010x\u2010y<\/jats:sub>Co<jats:sub>x<\/jats:sub>Mn<jats:sub>y<\/jats:sub>O<jats:sub>2<\/jats:sub>, NRNCM) as cathode materials for lithium\u2010ion batteries. Although the battery performance depends on the chemical heterogeneity during NRNCM calcination, it has not yet been elucidated. Herein, through synchrotron\u2010based X\u2010ray, mass spectrometry microscopy, and structural analyses, it is revealed that the temperature\u2010dependent reaction kinetics, the diffusivity of solid\u2010state lithium sources, and the ambient oxygen control the local chemical compositions of the reaction intermediates within a calcined particle. Additionally, it is found that the variations in the reducing power of the transition metals (i.e., Ni, Co, and Mn) determine the local structures at the nanoscale. The investigation of the reaction mechanism via imaging analysis provides valuable information for tuning the calcination chemistry and developing high\u2010energy\/power density lithium\u2010ion batteries.<\/jats:p>","DOI":"10.1002\/adma.202207076","type":"journal-article","created":{"date-parts":[[2022,12,30]],"date-time":"2022-12-30T08:44:52Z","timestamp":1672389892000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":69,"title":["Solid\u2010State Reaction Heterogeneity During Calcination of Lithium\u2010Ion Battery Cathode"],"prefix":"10.1002","volume":"35","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-2832-0343","authenticated-orcid":false,"given":"Sugeun","family":"Jo","sequence":"first","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1850-4701","authenticated-orcid":false,"given":"Jeongwoo","family":"Han","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3143-1079","authenticated-orcid":false,"given":"Sungjae","family":"Seo","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Oh\u2010Sung","family":"Kwon","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering Yonsei University  Seoul 120\u2010749 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6523-2548","authenticated-orcid":false,"given":"Subin","family":"Choi","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jin","family":"Zhang","sequence":"additional","affiliation":[{"name":"Stanford Synchrotron Radiation Lightsource SLAC National Accelerator Laboratory  Menlo Park CA 94025 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2379-8911","authenticated-orcid":false,"given":"Hyejeong","family":"Hyun","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Juhyun","family":"Oh","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"},{"name":"Department of Materials Science &amp; Engineering and Research Institute of Advanced Materials (RIAM) Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3783-997X","authenticated-orcid":false,"given":"Juwon","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7809-7912","authenticated-orcid":false,"given":"Jinkyu","family":"Chung","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8295-4331","authenticated-orcid":false,"given":"Hwiho","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemistry Seoul National University  1 Gwanak\u2010ro, Gwanak\u2010gu Seoul 08826 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jian","family":"Wang","sequence":"additional","affiliation":[{"name":"School of Energy and Environment City University of Hong Kong  Hong Kong Hong Kong SAR P. 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