Modular reactor for in situ X-ray scattering, spectroscopy and ATR-IR studies of solvothermal nanoparticle synthesis

Understanding the chemical processes that occur during the solvothermal synthesis of functional nanomaterials is essential for their rational design and optimization for specific applications. However, these processes remain poorly understood, primarily due to the limitations of conventional ex situ characterization techniques and the technical challenges associated with in situ studies, particularly the design and implementation of suitable reactors. Here, we present a versatile reactor suitable for in situ X-ray scattering, X-ray spectroscopy and infrared spectroscopy studies performed during solvothermal synthesis under autoclave-like, inert conditions. The reactor enables precise control of the temperature between −20°C and 200°C, pressure up to 8 bar, magnetic stirring, and injection of gas or liquids. The reactor's capabilities are demonstrated by comprehensively studying the solvothermal synthesis of magnetite nanoparticles from iron acetyl­acetonate in benzyl alcohol through in situ X-ray scattering and spectroscopy, and attenuated total reflection infrared (ATR-IR) spectroscopy.