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Herein we report on the synthesis of a metastable (Cr,Y)2AlC MAX phase solid solution by co‐sputtering from a composite Cr–Al–C and elemental Y target, at room temperature, followed by annealing. However, direct high‐temperature synthesis resulted in multiphase films, as evidenced by X‐ray diffraction analyses, room‐temperature depositions, followed by annealing to 760°C led to the formation of phase...