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Traditional ex situ characterization techniques, however, capture only static snapshots and often introduce artifacts by disrupting the material's original state. In contrast, advanced in situ characterization techniques enable real\u2010time, non\u2010destructive monitoring of dynamic evolution in crystal structure, morphology, and chemical states under operating conditions. This review systematically summarizes the principles and recent progress of key in situ techniques\u2014including X\u2010ray diffraction, X\u2010ray photoelectron spectroscopy, X\u2010ray absorption spectroscopy, neutron diffraction, nuclear magnetic resonance, transmission electron microscopy, electrochemical impedance spectroscopy, Raman spectroscopy, infrared spectroscopy, electron paramagnetic resonance, and differential electrochemical mass spectrometry. We analyze their applications across three critical aspects: cathode material synthesis, lithium\u2010ion deintercalation mechanisms, and failure mechanisms. Furthermore, we discuss emerging strategies of multi\u2010technique integration and artificial intelligence (AI)\u2010assisted data analysis, which offer transformative potential for deciphering complex physicochemical processes. This multi\u2010technique collaborative paradigm provides new insights and pathways for overcoming current performance bottlenecks and accelerating the development of high\u2010energy, long\u2010life lithium\u2010ion battery cathodes.<\/jats:p>","DOI":"10.1002\/smll.74917","type":"journal-article","created":{"date-parts":[[2026,8,3]],"date-time":"2026-08-03T08:11:46Z","timestamp":1785744706000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["From Synthesis to Failure: In Situ Characterization of Lithium\u2010Ion Battery Cathodes"],"prefix":"10.1002","volume":"22","author":[{"given":"Xiaoyu","family":"Zhao","sequence":"first","affiliation":[{"name":"College of Chemistry and Materials Science Key Laboratory of Analytical Science and Technology of Hebei Province Hebei University  Baoding People's Republic of 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