In situ monitoring of the synthesis of precursors for battery active materials under controlled hydrodynamic conditions

To meet environmental objectives, one of the main levers is the electrification of the vehicle fleet. This will lead to a sharp increase in the production of Li-ion batteries over the next decade. For environmental and geostrategic reasons, recycling these batteries in Europe will have to be set up. Closed-loop recycling will require the synthesis of new cathode active materials (CAMs) from metals extracted from recycled battery leachates. CAMs are lamellar mixed oxides LiNixMnyCozO2. They are synthesized in two stages: i) co-precipitation and ii) calcination. NixMnyCoz(OH)2 transition metal hydroxide precursors are synthesized during co-precipitation, while their lithiation and oxidation are carried out during calcination. The physico-chemical properties of CAMs, and hence their electrochemical performance, are mainly determined during co-precipitation. In-depth mastery of the synthesis process is therefore essential to achieve the desired final properties. 
The aim of this thesis is to set up tools and associated characterizations enabling in situ monitoring of the various mechanisms (nucleation, growth, aggregation) under controlled hydrodynamic conditions. More specifically, it will involve to:
•    Develop a millifluidic reactor to control hydrodynamic conditions during synthesis,
•    Use the reactor for in situ synchrotron X-ray monitoring (WAXS, SAXS) of the structural and morphological properties of the particles,
•    Identify the different mechanisms involved in co-precipitation process and determine their respective influence on particle properties and kinetics.
These data will be used to feed models that will be invaluable aids in the design and management of the synthesis process.

Keywords: Battery, NMC, synthesis, materials, precipitation, characterization, X-ray

• Academic supervisor    Dr Clémence NIKITINE, IFPEN, ORCID : 0000-0003-2642-4349
• Doctoral School    206 - Ecole doctorale Chimie, Procédé, Environnement
• IFPEN supervisor    Dr Séverine HUMBERT, ORCID : 0000-0003-1884-2858
• PhD location    IFP Energies nouvelles, Lyon, France
• Duration and start date    3 years, starting in the fourth quarter 2024 (Novembre 4)
• Employer    IFPEN
• Academic requirements    University Master degree in chemistry or material engineering    
• Language requirements    English level B2 (CEFR), French level A2    
• Other requirements    Strong knowledge of characterization techniques and precipitation synthesis is required.

To apply, please send your cover letter and CV to the IFPEN supervisor indicated below.