Effect of milling and compaction on sintering of porcelain stoneware tiles

The present study aims to provide a deeper understanding of how different particle size distributions and degrees of powder compaction affect the densification process of porcelain stoneware tiles. For this purpose, three different batches underwent a laboratory simulation of the industrial tilemaking process, at growing grinding time or increasing forming pressure, with technological characterization of both unfired and fired products. Sintering behaviour was determined by hot-stage microscopy. Phase composition was determined by XRD-Rietveld allowing the estimation of the chemical composition and physical properties of the liquid phase. The results illustrate the impact of too fine (or too coarse) grain size on powder compaction, firing shrinkage, water absorption, efficiency of densification, sintering rate, stability at high temperature, and risk of anticipated overfiring (and similarly for too high or too low forming pressure). Simultaneous variation of particle size and forming pressure beyond usual standards induced changes in technological behaviour that in most cases compensate each other. Phase composition is moderately influenced by particle size and little by powder compaction. The vitreous phase mainly suffered from a decreasing degree of polymerization as the particle size became finer or the dry bulk density decreased. In case of insufficient grinding, too much residual feldspars caused improper composition and properties of the glassy phase, which resulted in lower efficiency of densification and slower sintering rate. Both the sintering kinetics and degree of densification depend on the timescale, i.e. the ratio of surface tension to viscosity (melt) and median particle size. Nevertheless, a low powder compaction can trigger a microstructural effect on sintering (improving both densification rate and efficiency) that may outweigh the timescale effect.