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The increasing importance of recycling makes the recovery of valuableelements from slags interesting, e.g., by the concept of engineered artificialminerals (EnAMs). In this concept, it is aimed for the formation of EnAMs,meaning phase(s) with a high content of the to-be-recovered element(s) fromslags of pyrometallurgical recycling processes. For this, understanding thephase constitution of the slag systems is of high importance. The systemMg-Mn-Al-O is a metal oxide slag subsystem from Li-ion battery recycling, thatis critical for the formation of spinel phases, which are competing phases tothe possible Li-containing EnAM phase LiAlO2. Here, the phase constitution wasinvestigated using a thin film materials library that covers the compositionspace (Mg14-69Mn11-38Al14-74)Ox. By means of high-throughput energy-dispersiveX-ray spectroscopy and X-ray diffraction, the formation of the spinel solidsolution phase was confirmed for a wide composition space. Increasingpreferential orientation of the spinel solid solution along (400) withincreasing Mg content was identified. X-ray photoelectron spectroscopy was usedto measure the near-surface composition of selected areas of the materialslibrary, and detailed peak fitting of the Mn 2p3/2 region revealed the Mnoxidation state to be a mixture of Mn2+ and Mn3+. For one measurement area ofthe materials library containing equal atomic amounts of Mg, Mn and Al,transmission electron microscopy showed that the approximately 420 nm-thickfilm consists of columnar spinel grains with Mg, Mn and Al being evenlydistributed. Based on these results, we suggest that the shown high likelihoodof spinel formation in slags might be influenced by controlling the Mnoxidation state to enable the formation of desirable EnAM phases.

High-throughput study of the phase constitution of the thin film system Mg-Mn-Al-O in relation to Li recovery from slags