Methods for synthesising Zr‐based MAX phases powder generally require high temperature and product processing such as milling, which can introduce impurities and high cost. A new method to syntheszse Zr3Al3C5 powder from Zr, Al, and C particles in NaCl‒KCl molten salt was reported. The effects of temperature, Al content, and type of carbon source on the formation of Al–Zr–C compounds were investigated. The results show that molten salt synthesis can be used to prepare Zr3Al3C5 powder at a low temperature. When additional Al was added to yield a Zr:Al ratio of 2:9 and resin carbon was used as the carbon source, the purity of the prepared Zr3Al3C5 reached 96%. ZrC is always present in the powder as an impurity, which is consistent with many commercial MAX phases.
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