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A high nickel content (&gt;80%) provides an attractive balance between high energy density, long lifetime, and low cost. Consequently, Ni\u2010rich layered oxides cathode active materials (CAMs) are in high demand, and the importance of LiNiO<jats:sub>2<\/jats:sub> (LNO) as limiting case, is hence paramount. However, achieving perfect stoichiometry is a challenge resulting in various structural issues, which successively impact physicochemical properties and result in the capacity fade of LIBs. To better understand defect formation in LNO, the role of the Ni(OH)<jats:sub>2<\/jats:sub>\u00a0precursor morphology in the synthesis of LNO requires in\u2010depth investigation. By employing aberration\u2010corrected scanning transmission electron microscopy, electron energy loss spectroscopy, and precession electron diffraction, a direct observation of defects in the Ni(OH)<jats:sub>2<\/jats:sub>\u00a0precursor preparedis reported and the ex situ structural evolution from the precursor to the end product is monitored. During synthesis, the layered Ni(OH)<jats:sub>2<\/jats:sub>\u00a0structure transforms to partially lithiated (non\u2010layered) NiO and finally to layered LNO. The results suggest that the defects observed in commercially relevant CAMs originate to a large extent from the precursors, hence care must be taken in tuning the co\u2010precipitation parameters to synthesize defect\u2010free Ni\u2010rich layered oxides CAMs.<\/jats:p>","DOI":"10.1002\/smll.202205508","type":"journal-article","created":{"date-parts":[[2022,11,26]],"date-time":"2022-11-26T14:42:55Z","timestamp":1669473775000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Probing the Ni(OH)<sub>2<\/sub> Precursor for LiNiO<sub>2<\/sub> at the Atomic Scale: Insights into the Origin of Structural Defect in a Layered Cathode Active Material"],"prefix":"10.1002","volume":"19","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7457-8839","authenticated-orcid":false,"given":"Anuj","family":"Pokle","sequence":"first","affiliation":[{"name":"Materials Science Center (WZMW) and Department of Physics Philipps\u2010University Marburg  35032 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4175-9278","authenticated-orcid":false,"given":"Daniel","family":"Weber","sequence":"additional","affiliation":[{"name":"Battery and Electrochemistry Laboratory Institute of Nanotechnology Karlsruhe Institute of Technology (KIT)  Hermann\u2010von\u2010Helmholtz\u2010Platz 1 76344 Eggenstein\u2010Leopoldshafen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4034-7706","authenticated-orcid":false,"given":"Matteo","family":"Bianchini","sequence":"additional","affiliation":[{"name":"Battery and Electrochemistry Lab (BELLA) BASF SE  Carl\u2010Bosch\u2010Strasse 38 67056 Ludwigshafen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9221-4756","authenticated-orcid":false,"given":"J\u00fcrgen","family":"Janek","sequence":"additional","affiliation":[{"name":"Battery and Electrochemistry Laboratory Institute of Nanotechnology Karlsruhe Institute of Technology (KIT)  Hermann\u2010von\u2010Helmholtz\u2010Platz 1 76344 Eggenstein\u2010Leopoldshafen Germany"},{"name":"Institute of Physical Chemistry &amp; Center for Materials Research Justus\u2010Liebig\u2010University  Heinrich\u2010Buff\u2010Ring 17 35392 Giessen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4456-5439","authenticated-orcid":false,"given":"Kerstin","family":"Volz","sequence":"additional","affiliation":[{"name":"Materials Science Center (WZMW) and Department of Physics Philipps\u2010University Marburg  35032 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2022,11,26]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41560-021-00776-y"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acsami.8b04405"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1039\/C8CP03237H"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1149\/2.1381902jes"},{"key":"e_1_2_8_5_1","volume":"58","author":"Bianchini M.","year":"2018","journal-title":"Angew. 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