Reconstruction of the Wet Chemical Synthesis Process: The Case of Fe5C2 Nanoparticles

Wet chemical synthesis (WCS), especially under high temperatures, is one of the most frequently used strategies for nanostructured material construction, which has been used extensively in medical-, energy-, and environment-related applications. Although knowledge about the WCS process has been accumulated in the past two decades, the high temperature used in the process and multiphase nature of intermediates and products are key factors preventing the processes from rationalization. In this paper, by using multilevel in situ cells, we developed a strategy to monitor the reaction details of WCS processed in the solid, liquid, and gas phase simultaneously. This protocol has proven successful to reconstruct the WCS process of Fe5C2 nanoparticles (NPs) and unravel the complicated chemistry in the synthesis process.