Freeze-Lining Formation of a Synthetic Lead Slag: Part I. Microstructure Formation

Abstract

Recently, freeze linings have been selected more frequently to protect pyrometallurgical reactor walls, due to a number of advantages over conventional refractory linings, such as a self-regenerating capability and the possibility of operating under high-intensity process conditions. A freeze lining is formed on a cooled reactor wall in a time-dependent temperature gradient. A full description of freeze-lining development, including phase formation as a function of temperature, time, and position, is important in understanding freeze-lining formation mechanisms and may be instrumental for the design of a sustainable freeze-lining concept. Freeze-lining formation is therefore investigated in a synthetic lead slag system: PbO-FeO-Fe2O3-ZnO-CaO-SiO2. Lab-scale freeze linings were produced by submerging an air-cooled probe into liquid slag for different times ranging from 1 to 120 minutes. The freeze-lining microstructures were characterized with optical microscopy, scanning electron microscopy (SEM), and electron probe X-ray microanalysis. The results were compared with the results of reference experiments. The freeze-lining formation of the studied slag system is initially dominated by the formation of glass and a highly viscous liquid. After 1 minute, extensive crystallization occurs and further growth of the freeze lining is determined by the growth of the melilite phase, which forms networking crystals. Because the heat transfer occurs very quickly, these melilite crystals form in undercooled liquid. Because the initial solidification rate is high, mass exchange between the freeze lining and bath affects the freeze-lining growth only when the freeze lining almost reaches its steady-state thickness.