The effects of process parameters on iron nanoparticle formation and properties while using ferrocene as a precursor in a low-pressure capacitively coupled plasma are investigated. The L18 array of the Taguchi method, followed by the L4 array, is used with the notional objective of increasing the yield of nanoparticles. A study of the size, shape and composition of the particles (using transmission electron microscopy, high-resolution transmission electron microscopy, Raman spectroscopy, x-ray diffraction, CHON and inductively coupled plasma-atomic emission spectroscopy analysis) gives an insight into the role played by various process parameters. Pressure is the most critical parameter in increasing nanoparticle yield, whereas hydrogen flow plays a key role in determining the nanoparticle size and composition. Atomic hydrogen helps in removing amorphous carbon and reducing the nanoparticle size. RF power plays an important role in the dissociation of ferrocene thus also affecting the composition. Nanoparticles obtained using optimized conditions are a mixture of Fe3O4 and Fe2O3 with cluster size 25–40 nm in diameter that are further made up of 2–4 nm crystallites. Magnetic property measurements indicate that the nanoparticles are super-paramagnetic in nature.
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