Precipitation mechanism and microstructural evolution of Al2O3/ZrO2(CeO2) solid solution powders consolidated by spark plasma sintering

doi:10.1016/j.jmst.2019.09.028

Abstract

Abstract:

It is difficult to synthesize Al₂O₃/ZrO₂ solid solution because of its low solubility under equilibrium solidification conditions. In this work, a new combustion synthesis combined with water atomization (CS-WA) method was developed to prepare supersaturated Al₂O₃/ZrO₂(CeO₂) solid solution powders. The ultra-high cooling rate supplied by CS-WA greatly extends solid solubility of Al₂O₃ in ZrO₂. The precipitation mechanism of solid solution was investigated by systematic heat treatments. The initial temperature of the metastable phase decomposed into Al₂O₃ and ZrO₂ is 1050 °C, and it could be completely precipitated at 1400 °C in 0.5 h. The precipitated ZrO₂ particles were uniformly dispersed in Al₂O₃ matrix and grew into submicron scale at annealing temperature of 1450 °C. Subsequently, together with detailed microstructure, phase composition, as well as mechanical properties were collaboratively outlined to discuss spark plasma sintering (SPS) behavior. The solid solution precipitated Al₂O₃ matrix and ZrO₂ particles during the SPS process. Partial ZrO₂ particles were uniformly distributed within Al₂O₃ matrix, while the residuary ZrO₂ located at the grain boundaries and formed special transgranular/intergranular structure. The average size of nanoscale transgranular ZrO₂ particles was only ～11.5 nm. The compact ZrO₂ toughened Al₂O₃ nano ceramic (N-ZTA) exhibits excellent mechanical properties. This work provides a guidance to produce nanostructured ZTA with high performance.

Key words: Solid solution, Precipitation, Spark plasma sintering, ZTA, Transgranular/intergranular structure

Wanjun Yu, Yongting Zheng, Yongdong Yu. Precipitation mechanism and microstructural evolution of Al₂O₃/ZrO₂(CeO₂) solid solution powders consolidated by spark plasma sintering[J]. J. Mater. Sci. Technol., 2020, 41: 149-158.

Figures/Tables 12

Fig. 1. XRD pattern of the synthesized AZC solid solution powders.

Table 1 Lattice parameter of solid solution powders.

Sample	Peak 1 (2θ)	Peak 2 (2θ)	Peak 3 (2θ)	a (mm)	b (mm)	c (mm)
Pure t-ZrO₂	29.73°	49.28°	59.30°	0.365	0.365	0.531
AZC	30.32°	50.83°	60.37°	0.361	0.361	0.517

Fig. 2. Powder morphologies (a), particle-size distribution (b), cross-sectional microstructure (c) and EDS spectra (d) of the synthesized AZC solid solution powders.

Fig. 3. XRD patterns of AZC solid solution powders after annealing at 550-1450 °C.

Fig. 4. BSE images of AZC solid solution powders after annealing at 950-1450 °C: (a) AZC-950; (b) AZC-1050; (c) AZC-1150; (d) AZC-1250; (e) AZC-1350; (f) AZC-1450.

Fig. 5. Densification curves of AZC solid solution powders in the SPS (red curve: temperature; blue curve: displacement; green curve: shrinkage rate; black curve: pressure).

Fig. 6. BSE image of the N-ZTA ceramic.

Fig. 7. BF-TEM (a), HAADF-STEM at high magnification (b), HAADF-STEM at low magnification (c) and particle-size distribution (d) of transgranular ZrO2 particles.

Fig. 8. Corresponding EDS elemental mapping of Fig. 7(c): (a) O element; (b) Al element; (c) Zr element; (d) Ce element.

Fig. 9. (a) HRTEM image of the N-ZTA ceramic and (b-d) the magnified high-resolution images of I, II and III in (a), respectively. The grain boundaries (GB) is marked by the blue triangles. Insets are the corresponding FFT patterns.

Fig. 10. SEM micrographs of fracture surface for N-ZTA composite ceramic: (a, b) high magnification; (c, d) low magnification.

Fig. 11. XRD patterns of AZC powders and N-ZTA composite ceramic: (a) AZC-1400-0.5 h; (b) polished surface of N-ZTA; (c) fracture surface of N-ZTA.

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Precipitation mechanism and microstructural evolution of Al₂O₃/ZrO₂(CeO₂) solid solution powders consolidated by spark plasma sintering

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