Characterization of Black Mass and Leaching Residue during Recycling combining Microwave Digestion and XRD

Black mass from End-of-Life (EoL) lithium-ion batteries (LIB) is subjected to acid leaching in hydrometal-lurgical recycling, during which metal species are dissolved and a solid residue remains. For effective processing of black mass and optimal step design, detailed knowledge of its chemical and phase compo-sition is essential. The combined use of Multiwave 7501 for efficient microwave-assisted acid and XRDynamic 500 for XRD analysis provides an optimal characterization workflow to support and optimize LIB recycling.

The development of new energy storage concepts and the steady increase in electromobility are leading to a continuous rise in the number of End-of-Life (EoL) lithium-ion batteries (LIBs). As these batteries contain significant amounts of critical raw materials, such as lithium and cobalt, substantial efforts are being made to transition toward a circular economy for battery production, in which recycling plays a key role. A common first step in EoL battery recycling is the extraction of so-called black mass, typically achieved by shredding the batteries and removing the electrolyte as well as larger fragments of metals or polymers, resulting in a powdered material. This black mass serves as starting material for subsequent hydrometallurgical recycling during which it is commonly subjected to acid leaching as a first step, to extract the valuable metal components, leaving behind an indissoluble solid residue.

Investigations of the chemical and phase composition of the black mass, in comparison with that of the remaining solid residue, can provide valuable insight into the effectiveness of the leaching process. This knowledge can support the development of improved methods for black mass preparation and its subsequent recycling. In this application report, two analytical methods are employed:

  • Microwave-assisted acid digestion to ensure complete, residue-free dissolution of black mass samples, enabling accurate determination of metal contents by inductively coupled plasma optical emission spectroscopy (ICP-OES).
  • XRD to determine the crystalline phase of the black mass and the solid residue.

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