A versatile chemical vapor synthesis reactor for in situ x-ray scattering and spectroscopy

Rev Sci Instrum. 2022 Nov 1;93(11):113706. doi: 10.1063/5.0122461.

Abstract

We describe a versatile reactor system for chemical vapor synthesis of nanoparticles, which enables in situ investigations of high temperature gas phase particle formation and transformation processes by x-ray scattering and x-ray absorption spectroscopy. The system employs an inductively heated hot wall reactor as the energy source to start nanoparticle formation from a mixture of precursor vapor and oxygen. By use of a modular set of susceptor segments, it is especially possible to change solely the residence time of the gas mixture while keeping all other process parameters (temperature, gas flow, pressure) constant. Corresponding time-temperature profiles are supported by computational fluid dynamics simulations. The operation of the system is demonstrated for two example studies: tin oxide nanoparticle formation studied by small angle x-ray scattering and iron oxide nanoparticle formation by x-ray absorption spectroscopy.