Synthesis of Nano‐γ‐Ferric Oxide by Thermolysis of the 2‐Mercapto‐5‐Methylpyridine‐N‐Oxide‐Iron(III) Complex via Factorial Design

Abstract

2‐Mercapto‐5‐methylpyridine‐N‐oxide (MMPNO) and its sodium salt (NaMMPNO) were synthesized. The reaction of the latter with Fe3+ generates Fe(MMPNO)3 chelate. The thermolysis of this chelate at 350 °C yielded highly pure reddish‐brown γ‐Fe2O3 nanocrystallites with an average particle size of 6.2 nm, a particle size range of 4.2 to 14.8 nm, and a specific surface area of 51.5 m2g–1. The thermolysis process was optimized using the 22 fractional design. Quantitative tests and characterization of products were carried out by UV‐vis spectroscopy, XRD, LLS, SEM, TGA, BET, TEM, FT‐IR, elemental microanalysis, and classical analytical measurements.