Fabrication and modelling of Si3N4 ceramics with radial grain alignment generated through centripetal sinter-forging

doi:10.1016/j.jmst.2022.02.036

Abstract

Abstract:

Silicon nitride (Si₃N₄) based ceramics are one of the most attractive advanced engineering materials, which have been widely used under high-speed rotational operation or for mechanical contacts across a curved surface. In the present study, rotationally symmetric texturing of Si₃N₄, with radial grain alignment, was obtained by centripetal sinter-forging (CSF) of a partially sintered sample. The average values of the included angles between the c-axis of the local Si₃N₄ grain and radial direction were approximately 16.4° and 11.0°, on the section plane perpendicular to the pressing direction, and parallel to both the pressing and radial directions, respectively. The compressive strain in the pressing direction forced the ceramic body to flow towards the central axis, resulting in compressive strain in the tangential direction and tensile strain in the radial direction. A fundamental physical model was created to simulate the grain rotation during the 3-dimentional strain reorientation, which revealed the rod-like grain would preferentially rotate toward the center of the sample under the CSF process. In addition, due to the friction between the sample surface and the pressing punch, the increased shear strain could enhance the Si₃N₄ grain alignment. Consequently, ceramics with rod-like grains perpendicular to the curved side surface could be anticipated by applying the centripetal forming concept in a controlled manner.

Key words: Si₃N₄ ceramic, Texture, Radial grain alignment, Modeling, CSF

Da-Wang Tan, Zhen-Yong Lao, Wei-Ming Guo, Akira Kondo, Takahiro Kozawa, Makio Naito, Kevin Plucknett, Hua-Tay Lin. Fabrication and modelling of Si₃N₄ ceramics with radial grain alignment generated through centripetal sinter-forging[J]. J. Mater. Sci. Technol., 2022, 126: 1-14.

Figures/Tables 17

Fig. 1. Schematic representations of: (a) the pre-sintering step, (b) the CSF process, (c) the conventional sinter-forging approach, and (d) the relative orientations of the surfaces, and grain angles that were examined after sinter-forging.

Fig. 2. Schematic diagram for the strength testing orientations, with: (a) the fracture plane orthogonal to the centripetal direction, and (b) the fracture plane parallel to the centripetal direction.

Fig. 3. Representative XRD patterns for: (a) the precursor powder mixture (α-Si3N4 plus sintering additives), and (b) the partially densified, disc-shaped sample.

Fig. 4. XRD patterns for the CSF ceramic, recorded from: (a) the SO surface, (b) the SPP surface, and (c) the SPO surface, (d) the JCPDS standard data for β-Si3N4, with the expected peak intensities shown for an isotropic scenario.

Fig. 5. Representative SEM image of the etched microstructure of the partially sintered sample after pre-sintering.

Fig. 6. Representative SEM images of the microstructures of the CSF processed β-Si3N4 ceramics on: (a) the SO plane, (b) the SPP plane, and (c) the SPO plane, (d) SEM image of the microstructure of an SO equivalent surface for a conventionally sinter-forged sample, as a comparison. The arrows point at the centripetal direction in each case.

Fig. 7. Distribution of the grain inclination angle values on: (a) the SO plane, and (b) the SPP plane of the CSF ceramic, (c) distribution of the grain inclination angle values on the SO plane of the conventionally sinter-forged β-Si3N4 ceramic, (d) the distribution of grain diameters measure on the SPO plane.

Table 1. The measured Vickers hardness, indentation fracture toughness, and flexural strength in each of the different orientation directions.

Hardness type	Vickers hardness (GPa)	Toughness type	Indentation toughness (MPa·m^0.5)	Strength type	Flexural strength (MPa)
On SO plane	17.01 ± 0.31	SO-PC	4.69 ± 0.32	Type O	1264 ± 66
	17.01 ± 0.31	SO-OC	6.96 ± 0.34	Type P	846 ± 54
On SPP plane	16.58 ± 0.20	SPP-PC	4.06 ± 0.23
	16.58 ± 0.20	SPP-OC	7.53 ± 0.41
On SPO plane	15.85 ± 0.27	SPO-PP	5.70 ± 0.13
	15.85 ± 0.27	SPO-OP	5.06 ± 0.33

Fig. 8. Outline of different types of toughness in different directions.

Fig. 9. Morphology of: (a) a Vickers indentation on the SPP plane, (b) crack propagation parallel to radial direction on the SPP plane, (c) crack propagation orthogonal to radial direction on the SO plane, and (d) crack propagation on the SPO plane.

Fig. 10. Schematic representation of the micro- and macrostructure development of CSF samples prepared with rod-like grains.

Fig. 11. Fundamental physical model of: (a) the three-dimensional size variations of the sample during CSF, and (b) the Euler angles of a grain in the Cartesian coordinate system, where the long axis of the grain coincides with the X axis.

Fig. 12. The variations of: (a) the difference between ϕ?f and ϕ?i with ϕ?i, (b) θ?f with ϕ?, with ε = -0.55, Kt = -0.6, and Kr = 1.6, as experimental conditions.

Fig. 13. Predicted grain angles at the local position in the deformation, with ε = -0.55, Kt = -0.6, and Kr = 1.6, for: (a) random initial angles, (b) the distribution of initial angles between the grain long axis orientation and radial direction, (c) the alignment angles for the final state material, and (d) the distribution of final angles between the grain and radial direction.

Fig. 14. Predicted aligned angles of the local grain in final state, with ε = -0.55, Kt = -0.6, and Kr = 1.6, for: (a) the variation of θ?SOf with different ϕ?f and θ?f, (b) the distribution of θ?SOf, (c) the variation of θ?SPPf by different ϕ?f and θ?f, and (d) the distribution of θ?SPPf.

Fig. 15. Illustrations of: (a) the shear strain observation procedure, with a laser cut path marked within the partially sintered compact, and (b) the laser marked path observed from SPP plane of the sample after CSF, as well as a representation of the velocity variation and grain rotation at different positions within the sample.

Fig. 16. Radially textured structural application concepts, utilizing rod-like grains oriented perpendicular to the outer surface.

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Fabrication and modelling of Si₃N₄ ceramics with radial grain alignment generated through centripetal sinter-forging

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