Synthesis and in vacuo deposition of iron oxide nanoparticles by microplasma-assisted decomposition of ferrocene

Abstract

Microplasma-assisted gas-phase nucleation has emerged as an important new approach to produce high-purity, nanometer-sized, and narrowly dispersed particles. This study aims to integrate this technique with vacuum conditions to enable synthesis and deposition in an ultrahigh vacuum compatible environment. The ultimate goal is to combine nanoparticle synthesis with photoemission spectroscopy-based electronic structure analysis. Such measurements require in vacuo deposition to prevent surface contamination from sample transfer, which can be deleterious for nanoscale materials. A homebuilt microplasma reactor was integrated into an existing atomic layer deposition system attached to a surface science multi-chamber system equipped with photoemission spectroscopy. As proof-of-concept, we studied the decomposition of ferrocene vapor in the microplasma to synthesize iron oxide nanoparticles. The injection parameters were optimized to achieve complete precursor decomposition under vacuum conditions, and nanoparticles were successfully deposited. The stoichiometry of the deposited samples was characterized in situ using X-ray photoelectron spectroscopy indicating that iron oxide was formed. Additional transmission electron spectroscopy characterization allowed the determination of the size, shape, and crystal lattice of the particles, confirming their structural properties.

Plasma oxidation of liquid precursors for complex metal oxides.

“…Studies involving inductively coupled plasma for droplet-to-particle concept has been successful but only shown with single component systems [25][26] . Schaefer and co-workers 27 studied the gas phase nucleation and in vacuo deposition of iron oxide nanoparticles from ferrocene vapor in a microplasma reactor. The difficulties inherent in vapor phase nucleation are lack of precise compositional control in making multi-metal oxides.…”