4.7 Article

Molten salt synthesis and formation mechanism of Ti3AlC2: A new path from Ti2AlC to Ti3AlC2

Journal

JOURNAL OF THE AMERICAN CERAMIC SOCIETY
Volume 106, Issue 9, Pages 5567-5579

Publisher

WILEY
DOI: 10.1111/jace.19178

Keywords

formation mechanism; max phases; phase transition; synthesis; transmission electron microscopy

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In this study, fine, pure Ti3AlC2 powder was prepared via Ti3Al alloy and carbon black under mild conditions with the assistance of molten salts. The results of X-ray diffraction, scanning electron microscopy, TG-DSC, and transmission electron microscopy (TEM) characterizations showed that high purity, nanosized Ti3AlC2 could be obtained at 900 degrees C with a 1:1 salt-to-material ratio. Further TEM investigations revealed the formation mechanism of Ti3AlC2 through the alloy raw material and the distinct path of the phase transition.
Fine, pure Ti3AlC2 powder is prepared in a very mild condition via Ti3Al alloy and carbon black with the assistance of molten salts. X-ray diffraction, scanning electron microscopy, TG-DSC, and transmission electron microscopy (TEM) characterizations show that the high purity, nanosized Ti3AlC2 can be obtained at 900 degrees C with the 1:1 salt-to-material ratio. The formation mechanism of Ti3AlC2 through this strategy of alloy raw material is fully studied under further TEM investigations, showing that the reaction process can basically be described as Ti3Al and C -> TiAl and TiC -> Ti2AlC and TiC -> psi and TiC -> Ti5Al2C3 and TiC -> Ti3AlC2, where the key psi, a modulated Ti2AlC structure, is determined for the first time containing alternate-displacement Al layers along (0 0 0 2) of Ti2AlC phase with a distinct selected area electron diffraction pattern. Such alternant displacement is considered a precondition of forming Ti5Al2C3 through topotactic transition, followed by Ti5Al2C3 converting into Ti3AlC2 by the diffusion of Ti, C atoms in the outside TiC. Several parallel orientations can be observed through the phase transition process: Ti2AlC (0 0 0 2)//psi (0 0 0 1), psi (0 0 0 1)//Ti5Al2C3 (0 0 0 3), Ti5Al2C3 (0 0 0 3)//Ti3AlC2 (0 0 0 2). Such parallel orientations among these phases apply an ideal condition for the topotactic reaction. The distinct path of the phase transition brings a significant change of heat effect compared with the traditional method, leading to a fast reaction rate and a mild reaction condition.

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