# Microwave-Assisted Rapid Synthesis of Metallic Iron Nanoparticles from Triiron Dodecacarbonyl

## TL;DR

This paper presents a fast and efficient microwave method to synthesize pure iron nanoparticles using a specific iron complex and a coating agent.

## Contribution

The novel contribution is a rapid microwave-assisted synthesis of Fe(0) nanoparticles with DDA coating, overcoming dissolution and purity issues.

## Key findings

- Fe(0) nanoparticles with FCC structure were synthesized rapidly using microwave and DDA coating.
- The synthesis method produced well-dispersed nanoparticles with consistent size and minimal oxidation.
- Surface coating with DDA was confirmed using ADF-STEM, FT-IR, and TGA.

## Abstract

Zero-valent iron (Fe(0)) nanoparticles have a wide range of applications, including catalysis, energy storage, and even reported roles in human neurochemistry. This study demonstrated that [Fe3(CO)12] dissolves in N,N-Dimethylformamide (DMF) within a minute to resolve the dissolution problem of this complex. Dodecylamine (DDA) was used to produce DDA-coated Fe(0) at 383 K in 30 s with a microwave reactor. The powder X-ray diffraction (PXRD) of the Fe(0) profile indicated a pure-phase face-centred cubic (FCC) structure with Fm3¯m space group. Varying the synthesis time from 30 s to 5 min did not significantly affect the unit cell parameters (3.5276 (±0.0001) and 3.5391 (±0.0001) Å). Microwave use yielded well-dispersed, pure Fe(0) nanoparticles, and the particle size, shape, elemental analysis, and surface oxidation of the Fe(0) nanoparticles were studied using scanning electron microscopy and dispersive X-ray spectroscopy (SEM/EDX). Annular Dark-Field Scanning Transmission Electron Microscopy (ADF-STEM) and Fourier-transform infrared (FT-IR) spectroscopy confirmed the surface coating of Fe(0) nanoparticles with DDA. Thermogravimetric analysis (TGA) was used to demonstrate the surface adsorption of DDA on Fe(0) nanoparticles. In addition, STEM showed that the average nanoparticle size under the stated synthesis conditions was 25.7 nm. This comparatively straightforward procedure offers advantages over existing practical approaches to the synthesis of Fe(0) nanoparticles, including safety, speed and reaction control.