Development, Testing and Validation of Recycling Solutions for Cathode and Black Mass at Lab Scale

As part of the FREE4LIB project, researchers are developing and testing innovative recycling technologies to give new life to materials from end-of-life lithium-ion batteries. The main goal is to recover valuable resources from used batteries and reintroduce them into the production chain, building the foundation for a more circular and sustainable European battery ecosystem.

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Context and objective of the deliverable

This deliverable gathers the results of laboratory-scale experiments designed to test different recycling solutions for black mass and cathode materials, two critical components of spent batteries.

The objective was to evaluate several recycling routes and identify the most effective ones for recovering high-value metals such as lithium, nickel, cobalt, and manganese, while minimizing environmental impact.

Three complementary approaches were explored :

• Hydrometallurgical process (acid leaching to recover metals),
• Combined pyro-hydrometallurgical process (thermal + chemical treatment to recover lithium and other metals),
• Direct cathode recycling (regenerating used materials for immediate reuse).

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Key findings

The results demonstrate significant progress in sustainable metal recovery and cathode regeneration

• Two    types of black mass were tested, showing that pyro-hydrometallurgical treatment offers strong potential, particularly for the selective recovery of lithium carbonate (Li₂CO₃).
• Several recycled compounds (including metal oxides, carbonates, and oxalates) were successfully transformed into precursors ready to be used for new cathode materials.
• A novel process using Natural Deep Eutectic Solvents (NADES) achieved outstanding recovery rates:100% cobalt, 99.9% manganese, 99.7% nickel, and 53% lithium,  all above the EU’s latest recycling targe
• Direct  cathode recycling via hydrothermal and electrochemical re-lithiation successfully restored the crystalline structure of degraded cathodes, allowing them to regain performance like fresh materials.

These findings confirm the feasibility of reusing recovered materials within the battery value chain and represent a major step towards industrial application.

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Recommendations and next steps

The deliverable confirms that several recycling routes are both technically viable and environmentally sound.

Next steps will focus on:

• Validating the use of recovered materials (nickel, cobalt, manganese oxalates, cobalt     sulfate, lithium salts) as precursors for new battery cells,
• Optimizing process conditions for large-scale implementation,
• Scaling up the most promising recycling technologies in Work Package 4, moving from laboratory success to industrial demonstration.

Ultimately, these advances bring Europe closer to a circular, low-impact battery industry, reducing dependence on imported raw materials and supporting the transition toward sustainable mobility.

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You can read the full deliverable here