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X\u2010ray diffraction, nitrogen adsorption, scanning electron microscopy, and transmission electron microscopy with energy\u2010dispersive X\u2010ray, and X\u2010ray photoelectron spectroscopy analyses revealed the formation of nanoscale layered structures, which enhanced specific surface areas (approximately 20\u2005m<jats:sup>2<\/jats:sup>\/g) in the intermetallic compounds. In the initial deoxidation stage, Li<jats:sub>2<\/jats:sub>TiO<jats:sub>3<\/jats:sub>\u2010like compounds were observed as an intermediate, suggesting the substitution of M in MTiO<jats:sub>3<\/jats:sub> by Li from the molten LiCl. Compound MTiO<jats:sub>3<\/jats:sub> has a layered structure perpendicular to the <jats:italic>c<\/jats:italic> axis of the trigonal structure, suggesting that the layered structures may originate from the crystal structure of the precursors. Formation of the Li<jats:sub>2<\/jats:sub>TiO<jats:sub>3<\/jats:sub>\u2010like intermediate may help maintain the original layered structure during deoxidation and the subsequent alloying at temperatures as low as 600\u2009\u00b0C.<\/jats:p>","DOI":"10.1002\/chem.202300194","type":"journal-article","created":{"date-parts":[[2023,3,16]],"date-time":"2023-03-16T23:28:33Z","timestamp":1679009313000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Intermetallic Compound TiM (M=Co, Fe) with a Layered Structure Prepared by Deoxidizing Ilmenite\u2010type Oxides in Molten LiCl\u2010CaH<sub>2<\/sub> Mixtures"],"prefix":"10.1002","volume":"29","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-5438-321X","authenticated-orcid":false,"given":"Yasukazu","family":"Kobayashi","sequence":"first","affiliation":[{"name":"Renewable Energy Research Center National Institute of Advanced Industrial Science and Technology  2-2-9 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