Investigation of phase formation and phase constitution in the systems Li-Mg-Al-O and Li-Al-Mn-O with special focus on spinel solid solutions

本项目的目的是详细研究与锂离子电池回收相关的复合氧化物渣系(Li，Mg，Al，Si，Ca，Mn)-O中两个四元体系Li-Mg-Al-O和Li-Al-Mn-O的相形成。将特别关注尖晶石固溶体作为早期结晶形成LiAlO2的同时过程。这些子系统的研究将使用薄膜材料库的组合沉积进行，同时进行成分和晶体高通量表征以及矿物学调查和表征。在含锰的体系中，将特别关注形态(MnII-MnIV)对相反应的影响。将在相关温度下对材料库进行热处理，以获得有关体系相形成和动力学行为的信息。其结果将是两个多元氧化物系统的存在图。这种方法旨在为固化实验指定“感兴趣区域”。用X射线衍射仪和电子探针分析了Li，Mg，Al，Mn，O系统中的化合物和选定的凝固熔体的形貌。样品中的锂含量将使用XPS和SIMS进行分析，对于选定的样品将使用原子探针断层扫描进行分析。这些结果将与材料库一起用于矿物学表征，包括比较微观尺度(薄膜材料库)和宏观尺度(熔融实验)上的反应，并应要求进行微升打印实验作为中间步骤，以收集关于这些体系动力学的更多信息。

The objective of this project is the detailed investigation of the phase formation in the two quaternary subsystems Li-Mg-Al-O and Li-Al-Mn-O, which are part of the complex oxide slag system (Li, Mg, Al, Si, Ca, Mn)-O, relevant for Li-ion battery recycling. A special focus will be on spinel solid solutions as concurring processes to the formation of LiAlO2 as early crystallization. The investigation of the subsystems will be conducted using combinatorial deposition of thin film materials libraries, accompanied by compositional and crystallographic high-throughput characterization as well as mineralogical investigation and characterization. In the system with Mn a special focus will be on the influence of the speciation (MnII – MnIV) on the phase reactions. Annealing of the materials libraries will be carried out at relevant temperatures to gain information about the phase formation and kinetic behavior of the systems. The result will be existence diagrams of the two multinary oxide systems. This approach aims on specifying “regions of interest” for solidification experiments. The compounds and the morphology of selected solidified melts in the system Li, Mg, Al, Mn, O will be analyzed with PXRD and EPMA. Li contents in the samples will be analyzed using XPS and SIMS and for selected samples with atom probe tomography,. These results in combination with the material libraries will be used for mineralogical characterization including a comparison of the reactions on the micro-scale (thin film material library) and the macro-scale (melt experiments) with pico-liter printing experiments as intermediate step on demand to gather additional information on the kinetics of these systems.