Characterization of Black Mass and Leaching Residue during Hydrometallurgical Recycling combining XRD and Microwave Digestion
Black mass from End-of-Life Lithium-Ion Batteries is acid-leached in hydrometallurgical recycling, dissolving metal species and leaving a solid residue. For the optimal design of the processing steps, detailed knowledge of its composition is essential. Using Anton Paar’s XRDynamic 500 for high-quality XRD and Multiwave 7501 for efficient microwave-assisted acid digestion provides an optimal workflow for detailed characterization of black mass and recycling intermediates.
Introduction
The development of new energy storage concepts, and the steady increase in electromobility leads to an ongoing rise in the number of End-of-Life (EoL) Lithium-Ion Batteries (LIBs). Since these batteries contain large amounts of critical raw materials such as Lithium and Cobalt, a concerted effort is made to move towards a circular economy of battery production, which necessarily includes recycling of the critical components. A common first step in EoL battery recycling is the extraction of so-called black mass, usually by shredding the batteries and removing electrolyte and larger shreds of metal or polymers to receive a powdered material. Black mass serves as starting material for subsequent hydrometallurgical recycling during which it is commonly leached in acids as a first step to extract the valuable metal components, leaving back an indissoluble solid residue.
Investigating the phase and chemical composition of the black mass and comparing it to the composition of the remaining solid residue can give insights into the effectiveness of the leaching process and help develop better methods for black mass preparation and further recycling. In this application report, two analysis methods are employed:
- X-ray diffraction (XRD) to determine the crystalline phase of the black mass and the solid residue.
- Microwave-assisted acid digestion to ensure complete and residue-free dissolution of black mass samples for accurate determination of metal contents via inductively coupled plasma optical emission spectroscopy (ICP-OES).
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