Microstructural Characterisation of Microwave Sintered Silicon Nitride Ceramics

1992 ◽  
Vol 287 ◽  
Author(s):  
Kevin P. Plucknett ◽  
David S. Wilkinson

The microstructure of a series of microwave sintered silicon nitride based ceramics have been assessed using a combination of optical microscopy/image analysis and analytical electron microscopy. Materials were studied as-received and after post-sinter hot-isostatic pressing. The grain size of microwave sintered materials was appreciably finer than conventionally processed ceramics of similar composition, although the mechanism involved is not clear. The as-received ceramics exhibited a reverse porosity gradient (with the highest porosity level at the surface) due to heat dissipation to the cooler surroundings during sintering. This also resulted in a small increase in the β′ grain aspect ratio close to the surface arising from an increase in the glass phase viscosity as the temperature decreases. Post-sinter HIPing of microwave sintered samples resulted in the elimination of most of the bulk porosity, but not near the surface. This is due to the reverse porosity gradient previously described, which leads to a transition from closed to open porosity with decreasing density near to the surface.

1995 ◽  
Vol 10 (6) ◽  
pp. 1387-1396 ◽  
Author(s):  
Kevin P. Plucknett ◽  
David S. Wilkinson

The microstructure of a microwave-densified silicon nitride based ceramic has been assessed in the as-sintered, post-sinter hot-isostatically pressed (HIPed) and annealed conditions. The grain size of the as-sintered material, which is a low substitution β′-Sialon, was significantly finer than observed in conventionally processed materials of similar composition. The as-sintered ceramic exhibits a reverse porosity gradient (with the highest porosity level at the surface) due to heat dissipation to the cooler surroundings during microwave processing. This also results in a higher β′ aspect ratio close to the surface arising from an increased glass viscosity (due to heat loss) and compositional change in this region during sintering. HIPing results in removal of all porosity from the sample core; however, a reduced porosity surface layer is retained. Significant β′-Sialon grain growth is also apparent after HIPing. A fine β′ grain structure was retained after annealing, with partial devitrification of the glassy grain boundary phase to β-Y2Si2O7.


1996 ◽  
Vol 430 ◽  
Author(s):  
M. E. Brito ◽  
K. Hirao ◽  
M. Toriyama ◽  
M. Hirota

AbstractPreliminary results on microwave sintering of seeded silicon nitride show that a well defined bi-modal grain size distribution is attainable in Si3N4-Y2O3-Al2O 3-MgO sintered bodies by microwave sintering at 28 GHz of materials seeded with ß-Si3N4 particles (2 vol. %). A positive effect on the mechanical performance is anticipated for these microstructurally controlled silicon nitride ceramics


2007 ◽  
Vol 554 ◽  
pp. 107-112 ◽  
Author(s):  
V. Demir ◽  
Derek P. Thompson

Silicon nitride samples were pressureless sintered with up to 5 w/o MgO to give densities in the range 98-99% of theoretical. After pressureless sintering, selected samples were placed in a vacuum heat treatment furnace surrounded by a carbon bed in a carbon crucible at a pressure of less than 4x10-4 mbar, and vacuum heat treated at different temperatures and times to remove grainboundary glass. The results showed that this was substantially achieved at 1575oC for 3h and that increasing the time to 5 hours gave still further improvement. SEM images, EDX analysis and oxidation tests provided additional evidence for the removal of Mg from the samples.


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