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From spent alkaline batteries to ZnₓMn₃₋ₓO₄ by a hydrometallurgical route: synthesis and characterization

Romo, Lorena Alcaraz, López-Fernández, Ana, García-Díaz, Irene, Fernández, Paloma, Urbieta, Ana, López, Félix A.
RSC advances 2018 v.8 no.58 pp. 33496-33505
Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, batteries, coprecipitation, crystal structure, hydrochloric acid, leaching, magnetic properties, manganese, oxides, temperature, zinc
A series of Zn/Mn binary oxides with different molar ratios (1.4–11) were synthesized via co-precipitation from a solution obtained through the acidic (HCl) leaching of a black mass originating from the mechanical recycling of spent alkaline and Zn–C batteries. The oxides obtained were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Magnetic properties of the samples were also investigated. The Raman spectroscopy results showed all the binary metallic oxides belong to the ZnₓMn₃₋ₓO₄ (0.25 ≤ x ≥ 1.75) type. All showed a spinel crystalline structure. The saturation magnetization decreases with the Zn/Mn molar ratio; a maximum of 13.19 emu g⁻¹ was found for the molar ratio of 11 at the Curie temperature (25.5 K). XPS showed that all the synthesized compounds contained Mn²⁺, Mn³⁺ and Mn⁴⁺. Mn²⁺ was the most prominent at a molar ratio of 11, Mn³⁺ was most common at a molar ratio of 2, and Mn⁴⁺ at 1.4.