Densification and Phase Transformation in Multi-Layered Graded Si(3)N(4)–TiN Components Produced by Field-Assisted Sintering

The structural and/or functional design of multiphase ceramics, along with their processing, are timely research topics in the area of field-assisted sintering techniques, such as spark plasma sintering, especially for systems containing both electrically insulating and conductive phases. In the present study, spark plasma sintering of Si(3)N(4)–TiN composites was investigated by changing the TiN particle size and electrical current waveform. Their combined effects on both the densification behavior and α-to-β phase conversion of the Si(3)N(4) matrix was studied and compared by means of a thermodynamic approach and dilatometric measurements. Through the control of TiN phase characteristics and heating mode, double-layered Si(3)N(4)-based components were also prepared using a one-step spark plasma sintering process, which was compared with conventional hot-pressing. It was shown that the size of the conductive TiN phase has a significant influence on the particle rearrangement, with the formation of a liquid phase, and the solution–diffusion–precipitation process, through the field-induced local heating and electrowetting mechanisms. Moreover, the contribution of current pulsing to the densification and α-to-β conversion of the layered Si(3)N(4)-based components was mostly dependent upon the particle size distribution and content of the TiN phase, indicating that the electric-field effect is dependent upon current path.