(Ca,Sr,Ba)ZrO3: A promising entropy-stabilized ceramic for titanium alloys smelting

doi:10.1016/j.jmst.2020.05.033

Abstract

Abstract:

A novel entropy-stabilized (ES) (Ca,Sr,Ba)ZrO₃ ceramic has been designed and synthesized by pressureless sintering of CaZrO₃, SrZrO₃ and BaZrO₃ powders mixtures at 1450 °C, 1500 °C and 1550 °C for 3 h. X-ray diffraction, scanning electron microscopy and transmission electron microscopy analyses collectively indicate that a single solid solution is formed with a homogeneous distribution of metal elements after sintering at 1550 °C. The relative density and hardness of the ES (Ca,Sr,Ba)ZrO₃ ceramic sintered at 1550 °C are 97.79 % and 10.84 ± 0.33 GPa, respectively. This ES (Ca,Sr,Ba)ZrO₃ exhibits lower thermal conductivity from 373 K to 1073 K than their constituting zirconates, CaZrO₃, SrZrO₃ and BaZrO₃. Most importantly, the ES (Ca,Sr,Ba)ZrO₃ ceramic possesses good corrosion resistance to TiNi alloy melt and no distinct reaction layer exists between TiNi alloy and ES (Ca,Sr,Ba)ZrO₃ ceramic in the contact region. The combination of these properties indicates that ES (Ca,Sr,Ba)ZrO₃ ceramic is promising for use as a novel crucible material for the melting of titanium alloys.

Key words: Entropy-stabilized ceramics, (Ca,Sr,Ba)ZrO₃, Corrosion resistance, Pressureless sintering, Thermal conductivity

Shuaihang Qiu, Mingliang Li, Gang Shao, Hailong Wang, Jinpeng Zhu, Wen Liu, Bingbing Fan, Hongliang Xu, Hongxia Lu, Yanchun Zhou, Rui Zhang. (Ca,Sr,Ba)ZrO₃: A promising entropy-stabilized ceramic for titanium alloys smelting[J]. J. Mater. Sci. Technol., 2021, 65: 82-88.

Figures/Tables 10

Fig. 1. (a) XRD patterns of ES (Ca,Sr,Ba)ZrO3 prepared at different sintering temperatures and the mixture of starting materials, and (b) tetragonal perovskite crystal structure of (Ca,Sr,Ba)ZrO3.

Table 1 Crystal structure, lattice parameters and theoretical density of ES (Ca,Sr,Ba)ZrO3 and three constituent zirconates.

Materials	a (Å)	b (Å)	c (Å)	α=β=γ (°)	z	Symmetry	Space group	Theoretical density (g/cm³)
(Ca,Sr,Ba)ZrO₃	5.8229	5.8229	8.2333	90	4	Tetrahedral	I4/mcm	5.42
CaZrO₃	5.7558	8.0101	5.5929	90	4	Orthorhombic	Pnma	4.62
SrZrO₃	5.8140	8.1960	5.7920	90	4	Orthorhombic	Pnma	5.46
BaZrO₃	4.1930	4.1930	4.1930	90	1	Cubic	Pm-3m	6.23

Table 2 Bulk densities and relative densities of ES (Ca,Sr,Ba)ZrO3 sintered at different temperatures.

Sintering temperature (°C)	Bulk density (g/cm³)	Relative density (%)
1450	5.11	94.28
1500	5.28	97.42
1550	5.30	97.79

Fig. 2. SEM images of the fracture surface of ES (Ca,Sr,Ba)ZrO3 sintered at (a) 1450 °C, (b) 1500 °C and (c) 1550 °C.

Fig. 3. SEM micrographs of the polished surface and the corresponding EDS mapping of ES (Ca,Sr,Ba)ZrO3 sintered at (a) 1450 °C, (b) 1500 °C and (c) 1550 °C.

Fig. 4. (a) TEM image, (b) SAED pattern and (c) HRTEM image of ES (Ca,Sr,Ba)ZrO3 sintered at 1550 °C.

Fig. 5. HAADF image of grain boundary of triple point and the corresponding EDS mapping and line scanning across the grain boundary of ES (Ca,Sr,Ba)ZrO3 sintered at 1550 °C.

Table 3 Relative densities, Vickers hardness and room temperature thermal conductivities of ES (Ca,Sr,Ba)ZrO3, BaZrO3, SrZrO3 and CaZrO3.

Materials	Relative density (%)	Vickers hardness (GPa)	Thermal conductivity(W K^-1 m^-1)
ESC-1550 °C	97.79	10.84 ± 0.33	1.466 (31.0 °C)
ESC-1500 °C	97.42	12.16 ± 0.51	1.292 (30.9 °C)
ESC-1450 °C	94.28	10.24 ± 1.2	1.089 (30.6 °C)
BaZrO₃ [48]	∼98	11.10 ± 1.9	—
SrZrO₃ [48]	∼98	—	—
SrZrO₃ [49]	> 95	9.20 ± 0.1	—
CaZrO₃ [50]	97-98	8.42 ± 0.11	—
CaZrO₃ [51]	96.8	—	—
Rule of mixture (CaZrO₃, SrZrO₃, BaZrO₃)	—	9.57	—

Fig. 6. Comparison of thermal conductivities of ES (Ca,Sr,Ba)ZrO3 sintered at 1450 °C to 1550 °C with those of the three constituent zirconates [48,51] at different temperatures.

Fig. 7. (a) SEM micrograph of the interface between ES (Ca,Sr,Ba)ZrO3 and TiNi, and the corresponding EDS composition analysis on A point of TiNi side and B point of ES (Ca,Sr,Ba)ZrO3 side, (b) SEM image and EDS line scanning across the interface between the TiNi alloy and ES (Ca,Sr,Ba)ZrO3.

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(Ca,Sr,Ba)ZrO₃: A promising entropy-stabilized ceramic for titanium alloys smelting

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