{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,23]],"date-time":"2026-10-23T21:09:10Z","timestamp":1792789750197,"version":"4.5.0"},"reference-count":243,"publisher":"MDPI AG","issue":"19","license":[{"start":{"date-parts":[[2026,9,24]],"date-time":"2026-09-24T00:00:00Z","timestamp":1790208000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Science Committee of the Ministry of Science and Higher Education of the Republic of Kazakhstan","award":["AP23486690"],"award-info":[{"award-number":["AP23486690"]}],"id":[{"id":"https:\/\/ror.org\/05tyne317","id-type":"ROR","asserted-by":"crossref"}]},{"award":["AP23486690"],"award-info":[{"award-number":["AP23486690"]}],"id":[{"id":"https:\/\/ror.org\/05tyne317","id-type":"ROR","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Nanomaterials"],"abstract":"<jats:p>Binary Fe-containing LDHs and structurally related layered hydroxides are being widely investigated as adsorbents, catalysts, and redox-active nanomaterials. Yet, links among coprecipitation, phase formation, nanostructure, and reactive-site accessibility remain inconsistently interpreted. This critical review evaluates studies published mainly from 2015 to July 2026 on CoFe, NiFe, MgFe, ZnFe, MnFe, CuFe, and CaFe layered hydroxides and Fe(II)\/Fe(III) green rust. Coprecipitation is not a single standardized route: local supersaturation, reagent delivery, mixing, complexation, atmosphere, interlayer chemistry, and aging can alter metal incorporation and phase development, while Fe-rich transient precursors may participate under system-specific conditions. The commonly cited Fe(III) fraction of x = 0.20\u20130.33 is an empirical guideline rather than a universal stability window, and conventional M(II)-Fe(III) LDHs, CaFe hydrocalumite-\/AFm-related phases, and green rust require distinct crystal-chemical interpretations. Nominal composition and LDH-like diffraction cannot establish homogeneous cation incorporation or phase purity. In contrast, diffraction broadening, BET area, nanosheet dimensions, and XPS fitting do not provide stand-alone evidence of defects or accessible reactive sites. Progress toward predictive synthesis requires standardized reporting, system-specific synthesis\u2013composition\u2013phase maps, time-resolved studies, quantitative structure\u2013accessibility relationships, and recognition of as-synthesized, working, recovered, and regenerated materials as potentially distinct structural states, supported by uncertainty analysis, negative outcomes, and validation across laboratories.<\/jats:p>","DOI":"10.3390\/nano16191210","type":"journal-article","created":{"date-parts":[[2026,9,24]],"date-time":"2026-09-24T16:29:53Z","timestamp":1790267393000},"page":"1210","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["From Coprecipitation to Nanostructure: Formation, Morphology, and Reactive-Site Accessibility in Fe-Containing Binary Layered Double Hydroxides"],"prefix":"10.3390","volume":"16","author":[{"ORCID":"https:\/\/orcid.org\/0009-0003-5149-2957","authenticated-orcid":false,"given":"Alua","family":"Alikeyeva","sequence":"first","affiliation":[{"name":"Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, Almaty 050040, Kazakhstan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4641-6779","authenticated-orcid":false,"given":"Nurbolat","family":"Kudaibergenov","sequence":"additional","affiliation":[{"name":"Department of Chemistry, Kazakh National Women\u2019s Teacher Training University, Almaty 050000, Kazakhstan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kairzhan","family":"Shalmagambetov","sequence":"additional","affiliation":[{"name":"Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, Almaty 050040, Kazakhstan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0006-5444-4266","authenticated-orcid":false,"given":"Abzal","family":"Azimbay","sequence":"additional","affiliation":[{"name":"Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, Almaty 050040, Kazakhstan"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2026,9,24]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"5206","DOI":"10.1039\/D4CY00842A","article-title":"Manipulating anion intercalation into layered double hydroxide for alkaline seawater oxidation at high current density","volume":"14","author":"Wu","year":"2024","journal-title":"Catal. 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