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Título

Chemical vs. electrochemical extraction of lithium from the Li-excess Li1.10Mn1.90O4 spinel followed by NMR and DRX techniques

Autor Martínez, Sandra ; Sobrados, Isabel ; Tonti, D.; Amarilla, José Manuel ; Sanz Lázaro, Jesús
Fecha de publicación 13-ene-2014
EditorRoyal Society of Chemistry (Great Britain)
Citación Physical Chemistry Chemical Physics 16(7): 3282-3291 (2014)
ResumenLithium extraction from the Li-excess Li1.10Mn 1.90O4 spinel has been performed by chemical and electrochemical methods in aqueous and in organic media, respectively. De-lithiated samples have been investigated by XRD, SEM, TG, 7Li and 1H MAS-NMR techniques. The comparative study has allowed demonstrating that the intermediate de-intercalated samples prepared during the chemical extraction by acid titration are similar to those prepared by the electrochemical way in a non-aqueous electrolyte. LiMn2O4 based spinel with a tailored de-lithiation degree can be prepared as a single phase by controlling the pH used in chemical extraction. 7Li MAS-NMR spectroscopy has been used to follow the influence of the manganese oxidation state on tetra and octahedral Li-signals detected in Li-extracted samples. The oxidation of Mn(iii) ions goes parallel to the partial dissolution of the spinel, following Hunter's mechanism. Based on this mechanism, a generalized chemical reaction has been proposed to explain the formation of intermediate Li+ de-intercalated samples during acid treatment in aqueous media. By the 1H MAS NMR study, no evidence of Li-H topotactic exchange in the bulk of the acid treated material was found. This journal is © the Owner Societies 2014.
Versión del editorhttp://dx.doi.org/10.1039/C3CP54386B
URI http://hdl.handle.net/10261/93878
DOI10.1039/C3CP54386B
Identificadoresdoi: 10.1039/C3CP54386B
issn: 1463-9076
e-issn: 1463-9084
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