Synthesis and microstructural properties of zinc oxide nanoparticles prepared by selective leaching of zinc from spent alkaline batteries using ammoniacal ammonium carbonate

Two different precursors of zinc oxide were prepared via the ammoniacal ammonium carbonate leaching of the black mass obtained during the recycling of alkaline batteries. For a concentration of 0.1 mol/L of ammonium in the leaching solution, zinc basic carbonate, was obtained, while for higher ammonium concentrations (0.5 and 1 mol/L), zinc ammonium carbonate was the final product. These precursors were characterised by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA/DTG) and Scanning electron microscopy (SEM), and calcined to obtain ZnO. Raman spectroscopy, X-ray diffraction and Transmission electron microscopy (TEM) analysis of the resulting zinc oxide samples indicated a wurtzite hexagonal lattice with a parameter values ranging from 3.23 Å to 3.30 Å, and c parameter values from 5.18 Å to 5.21 Å (values close to typical). The room temperature photoluminescence spectra of the zinc oxide samples showed two main bands: a high energy UV-blue band centred at either 412 or 382 nm (depending on the NH concentration of the leaching solution used), and a green band centred at 527 nm. These emission bands are comparable to those reported for pure zinc oxide.
This work has supported by the Envirobat España S.L. and by the Spanish Ministerio de Economía y Competitividad MINECO (Projects MAT 2012-31959 and CSD2009-00013) and MINECO/FEDER (MAT2015-65274-R; 2016-2019), Ministry of Economy and Competitiveness for their Postdoctoral Junior Grants (Ref. FPDI-2013-16391) contracts co-financed by the European Social Fund. PhD. Ana López Fernández expresses her gratitude to the Comunidad de Madrid for their Technical Junior Grants (Ref. PEJ15/AMB/Al-0049) contracts co-financed by the European Social Fund.