Thermal Evolution of NiFe-NO3 LDH and Its Application in Energy Storage Systems

In this work, the performances of nickel iron layered double hydroxides (LDH) with the nitrate anion at the interlayer (NiFe-NO3) for the manufacture of anodes for lithium-ion batteries have been tested before and after its sintering at different temperatures. After synthesis, the material was thermally analyzed in a range 30–1250 °C, showing a mass loss occurring in three different consecutive steps leading to a total mass decrease of ~30 mass%. Following thermogravimetric analysis (TGA), four samples were prepared by annealing at four different temperatures: one of the four did not undergo a thermal treatment (NiFe-0), while the remaining three were annealed at 250 °C, 360 °C, and 560 °C for 6 h (NiFe-250, NiFe-360, and NiFe-560). All materials where completely characterized via FE-SEM, PXRD, and FT-IR. The pristine LDH material showed some structural and compositional changes for growing temperatures, starting from the typical turbostratic hexagonal structure through a mixture of amorphous metal oxides and finally to the stoichiometric oxides FeNi2O4 and NiO. The as-obtained materials were mixed with carbon black (C65) and sodium alginate and tested as electrodes in Swagelok half cells in LP30 vs. metallic Li to perform CV and GCPL analysis. The electrochemical tests showed that the performances of NiFe-0, both in terms of stability and specific capacity, are not so different from the one of the NiFe-560, even if the Ni mass% in the former is lower than in the NiFe-560. This phenomenon could be explained by assuming a combined mechanism of reaction involving both intercalation and conversion.