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J. Mater. Sci. Technol.  2020, Vol. 41 Issue (0): 149-158    DOI: 10.1016/j.jmst.2019.09.028
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Precipitation mechanism and microstructural evolution of Al2O3/ZrO2(CeO2) solid solution powders consolidated by spark plasma sintering
Wanjun Yu, Yongting Zheng*(), Yongdong Yu
National Key Laboratory of Science and Technology on Advanced Composites in Special Environments and Center for Composite Materials and Structures, Harbin Institute of Technology, Harbin 150080, China
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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     
Received:  29 June 2019     
Corresponding Authors:  Zheng Yongting     E-mail:  zhengyt@hit.edu.cn

Cite this article: 

Wanjun Yu, Yongting Zheng, Yongdong Yu. Precipitation mechanism and microstructural evolution of Al2O3/ZrO2(CeO2) solid solution powders consolidated by spark plasma sintering. J. Mater. Sci. Technol., 2020, 41(0): 149-158.

URL: 

https://www.jmst.org/EN/10.1016/j.jmst.2019.09.028     OR     https://www.jmst.org/EN/Y2020/V41/I0/149

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