Synthesis and characterization of nanosized Ti3AlC2 ceramic powder by elemental powders of Ti, Al and C in molten salt

doi:10.1016/j.jmst.2019.02.009

Abstract

Abstract:

A simple method to synthesize high-content ternary carbide Ti₃AlC₂ nanoparticles from Ti, Al, and C starting elemental powders without ball milling in NaCl-KCl molten salt was reported. The effects of mass ratio of the salt to starting materials, temperature, reaction time, and Al molar ratio on preparation of Ti₃AlC₂ were investigated. The Ti₃AlC₂ formation is dramatically influenced by temperature and mass ratio of the salt to raw materials: a higher temperature and higher mass ratio of the salt to raw materials are more preferable for Ti₃AlC₂ powder formation. Homogenous Ti₃AlC₂ powder with particle size of ~100 nm is synthesized by 3Ti/Al/2C starting elemental powders in NaCl-KCl molten salt at 900 °C for 10 h, 950 °C for 5 h, or 1000 °C for 2 h, respectively, when the mass ratio of the salt to 3Ti/Al/2C starting materials is 10:1.

Key words: Nanosized Ti₃AlC₂, Ternary carbide, Powder, Molten salt

Huijun Liu, Ying Wang, Lingxu Yang, Ruijia Liu, Chaoliu Zeng. Synthesis and characterization of nanosized Ti₃AlC₂ ceramic powder by elemental powders of Ti, Al and C in molten salt[J]. J. Mater. Sci. Technol., 2020, 37: 77-84.

Figures/Tables 7

Fig. 1. XRD patterns of samples synthesized at mass ratio of eutectic NaCl?KCl salt to 3Ti/Al/2C starting elemental powders of (a) 1:1 and (b) 10:1 at 950?°C for 5?h.

Fig. 2. SEM images of samples synthesized at the mass ratio of eutectic NaCl?KCl molten salt to 3Ti/Al/2C powders of (a) 1:1 and (b) 10:1 at 950?°C for 5?h, (c) higher magniﬁcation micrograph of the fiber of area A in Fig. 2(a) and (d) TEM image of the fiber and the corresponding SAED pattern shown in the inset.

Fig. 3. XRD patterns (A) and detailed XRD patterns (B) of samples synthesized at the mass ratio of the salt to 3Ti/Al/2C powders of 10:1 at different temperature for different times: (a) 700?°C, (b) 750?°C, (c) 800?°C, (d) 850?°C, (e) 900?°C, and (f) 950?°C for 5?h, (g) 1000?°C for 2?h.

Fig. 4. XRD patterns (A) and the detailed XRD patterns (B) of samples synthesized at the mass ratio of the NaCl?KCl molten salt to 3Ti/Al/2C powders of 10:1 at 900?°C for different times: (a) 1?h, (b) 2?h, (c) 5?h, (d) 10?h.

Fig. 5. XRD patterns (A) and the detailed XRD patterns (B) of samples obtained at the mass ratio of the NaCl?KCl molten salt to 3Ti/Al/2C powders of 10:1 at 950?°C for 5?h: (a) 3:0.9:2, (b) 3:1:2, (c) 3:1.1:2, (d) 3:1.2:2.

Fig. 6. (a) FE-SEM images of the prepared Ti3AlC2 powder from 3Ti/Al/2C starting elemental powders in NaCl?KCl molten salt at 1000?°C for 2?h. The inset in (a) shows the digital photograph of a glass bottle filled with the obtained Ti3AlC2 powder. (b) Higher magniﬁcation micrograph from area A. (c) Energy-dispersive X-ray spectroscopy analysis result of area A in Fig. 6(a). (d), (e), and (f) elemental mapping of titanium, aluminum, and carbon, respectively, in Fig. 6(a).

Fig. 7. TEM images (a, b) of the Ti3AlC2 powder obtained from 3Ti/Al/2C starting elemental powders in NaCl?KCl molten salt at 1000?°C for 2?h. The inset in (a) shows the Tyndall scattering e? ;ect for the suspension of Ti3AlC2 nanoparticles in deionized water. (c) TEM and (d) HRTEM images of the typical layer structure on the cross-section of the obtained Ti3AlC2 powder in area A in Fig. 7(b). (e) TEM and (f) HRTEM images of the layered atomic stacking on the surface of the obtained Ti3AlC2 powder. The inset in (f) shows the corresponding SAED pattern of Ti3AlC2.

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Synthesis and characterization of nanosized Ti₃AlC₂ ceramic powder by elemental powders of Ti, Al and C in molten salt

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