Fabrication of Ni sulfides by thermal sulfidation

Abstract

The microstructure of Ni sulfides prepared by thermal sulfidation of pure Ni and their dependence of fabrication parameters were investigated by means of scanning electron microscopy and X-ray diffractions. Sulfidation was made by isothermally annealing Ni with the sulfur in vacuum sealed glass ampoules at 673 K for 120 - 600s under the sulfur pressure of 100 and 220 kPa. The sulfide layers formed in the early stage were found to consist of spherical particles smaller than 0.5um, which were grown and agglomerated with increasing annealing temperature. Thickness of sulfides developed on Ni substrate was found to increase with increasing annealing time and sulfur pressure. It was also found that compositions of dominant Ni sulfides changed with varying annealing time. At the initial stage, only Ni3S2 sulfide was formed on pure Ni, which was tightly bonded to Ni substrate. On increasing annealing time, NiS sulfide was formed. On further increasing annealing time, NiS1.97 sulfide was formed, which always coexisted with NiS sulfide. A mechanism for sulfidation of Ni is proposed as follows: 3Ni + 2S -> Ni3S2, Ni3S2+S -> NiS, NiS + S -> NiS1.97.