Ti₂AlN belongs to a novel class of nanolaminated materials: the MAX Phases. Up to now, several approaches were used to synthesize MAX phases under bulk forms but their synthesis as thin films remains poorly documented. Two research groups recently demonstrated that Ti₂AlN thin films formation can be achieved by high temperature magnetron sputtering processes. Here, alternative approaches are described. The first one is a two-step technique based on the deposition of a TiAl/TiN multilayer followed by a thermal annealing. Multilayers were deposited by dual ion beam sputtering at room temperature. Theses samples were then annealed (600°C and 780°C) to allow atomic diffusion and Ti₂AlN formation. HRTEM observations and EELS spectra were recorded prior and after the thermal treatment. The progressive formation of Ti₂AlN during the annealing was evidenced both from in situ plane view TEM and XRD observations. Our results suggest that nitrogen diffusion into the TiAl sublayers allows the formation of the MAX phase whereas the Al atoms in excess presumably out diffuse towards the TiN sublayers where they are inserted as interstitials. The second approach consists in a direct formation of Ti₂AlN by plasma nitriding of TiAl bulk substrates or thin films deposited by magnetron sputtering onto Si and TiAl substrates at room temperature. TiAl bulk substrates and thin films were then exposed to nitrogen plasma at 900°C during 2 hours. HRTEM observations and XRD spectra reveal that this procedure allows the MAX phase formation whatever the substrate is. Of interest, TiN formation was never observed. Furthermore, XRD analysis shows that (0002) textured Ti₂AlN thin films are obtained when TiAl layers are nitrided. The Ti₂AlN formation by nitriding will be discussed on the basis of XRD, TEM but also glow-discharge spectrometry experiments.

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