Spark Plasma Sintering of High-Energy Ball-Milled ZrB2 and HfB2 Powders with 20vol% SiC

ZrB2 and HfB2 with incorporation of SiC are being considered as structural materials for elevated temperature applications. We used high energy ball milling of micron-size powders to increase lattice distortion enhanced inter-diffusion to get uniform distribution of SiC and reduce grain growth during Spark Plasma Sintering (SPS). High-energy planetary ball milling was performed on ZrB2 or HfB2 with 20vol% SiC powders for 24 and 48 hrs. The particle size distribution and crystal micro-strain were examined using Dynamic Light Scattering Technique and x-ray diffraction (XRD), respectively. XRD spectra were analyzed using Williamson-Hall plots to estimate the crystal micro-strain. The particle size decreased, and the crystal micro-strain increased with the increasing ball milling time. The SPS consolidation was performed at 32 MPa and 2,000°C. The SEM observation showed a tremendous decrease in SiC segregation and a reduction in grain size due to high energy ball milling of the precursor powders. Flexural strength of the SPS consolidated composites were studied using Four-Point Bend Beam test, and the micro-hardness was measured using Vickers micro-indenter with 1,000 gf load. Good correlation is observed in SPS consolidated ZrB2+SiC with increased micro-strain as the ball milling time increased: grain size decreased (from 9.7 to 3.2 μm), flexural strength (from 54 to 426 MPa) and micro-hardness (from 1528 to 1952 VHN) increased. The correlation is less evident in HfB2+SiC composites, especially in micro-hardness which showed a decrease with increasing ball milling time.