Large-scale synthesis of nickel sulfide micro/nanorods via a hydrothermal process

Rhombohedral-phase NiS micro/nanorods were synthesized on a large scale through a hydrothermal method using NiCl₂·6H₂O and thiourea crystals as starting precursors. Recrystallized thiourea was observed to play an important role in the formation of micro/nanosized rods and flower-like structures. The molar ratio and reaction temperature of the precursors influenced the morphology and phase of NiS products. Pure rhombohedral NiS micro/nanorods were obtained on a large scale when the molar ratio between NiCl₂·6H₂O and thiourea crystals was fixed at 2:1, and the mixture was heated at 250℃ for 5 h. Flower-like NiS nanostructures were formed when the molar ratio between NiCl₂·6H₂O and thiourea crystals was maintained at 1:1. The Raman and Fourier-transform infrared (FTIR) spectra of the as-prepared rhombohedral NiS micro/nanorods were collected, and their magnetic properties were investigated. The results showed that the FTIR absorption peaks of the as-prepared product are located at 634 cm^-1 and their Raman peaks are located at 216 and 289 cm^-1; the as-prepared NiS micro/nanorods exhibited weak ferromagnetic behavior due to the size effect.