A multi-analytical methodology for the characterization of industrial samples of spent Ni-MH battery powders

Abstract

A multi-analytical methodology is implemented to characterize several sieving fractions of industrial samples of Black Mass (BM) powders originating from the thermo-mechanical treatment of cylindrical and prismatic-type spent nickel metal-hydride (Ni-MH) batteries. Elemental analyses of 17 elements (including C and O) indicate that the elemental composition of the powders (greater than93 %wt) does not depend on the battery type nor on the sieving fraction. XRD analyses evidence several phases (including Ni, NiO, CeO₂ and C) but their quantification is not possible. Beyond these standard characterisations, magnetic susceptibility measurements demonstrate that the amount of metallic nickel versus nickel oxide increases with the sieving fraction, and that powders from prismatic-type batteries contain twice as much metallic nickel than cylindrical ones. Thanks to statistical analysis (based on clustering algorithms) of an electron probe µ-analysis (EPMA) compositional map, the complete methodology allows us to propose a full phase distribution for the BM particles. Three types of particles are identified and quantified. They originate from the partial oxidation of the battery components (anode active mass, anode current collector, cathode active mass and cathode current collector). The whole picture highlights the joint importance of battery ageing mechanisms, thermal deactivation and BM sieving steps on powder composition.

Keywords: Black Mass characterization; Clustering algorithms; Elemental mapping; Magnetic susceptibility; Ni-MH battery recycling; Thermal deactivation.