Densification and Phase Transformation in Multi-Layered Graded Si₃N₄-TiN Components Produced by Field-Assisted...

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 Si₃N₄-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 Si₃N₄ 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 Si₃N₄-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 Si₃N₄-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.