In situ studies on phase transitions of tris(acetylacetonato)-aluminum(III) Al(acac)3

Abstract

In situ investigations on the nucleation and crystallization processes are essential for understanding of the formation of solids. Hence, the results of such experiments are prerequisites for the rational synthesis of solid materials. The in situ approach allows the detection of precursors, intermediates, and/or polymorphs, which are mainly missed in applying ex situ experiments. With a newly developed crystallization cell, simultaneous in situ experiments with X-ray diffraction (XRD) and luminescence analysis are possible, also monitoring several other reaction parameters. Here, the crystallization of the model system tris(acetylacetonato)-aluminum(III) Al(acac)3 was investigated. In the time-resolved in situ XRD patterns, two polymorphs of Al(acac)3, the α- and the γ-phase, were detected at room temperature and the influence of the pH value onto the product formation was studied. Moreover, changes in the emission of Al(acac)3 and the light transmission of the solution facilitated monitoring the reaction by in situ luminescence. The first results demonstrate the potential of the cell to be advantageous for controlling and monitoring several reaction parameters during the crystallization process.