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We use transmission electron microscopy (TEM) for in situ studies of electron-beam-induced crystallization behavior in thin films of amorphous transition metal silicon carbides based on Zr (group 4 element) and Nb (group 5). Higher silicon content stabilized the amorphous structure while no effects of carbon were detected. Films with Nb start to crystallize at lower electron doses than the Zr-containing ones. During the crystallization, equiaxed MeC grains are formed in all samples with larger grains for ZrC (∼5 nm) compared to NbC (∼2 nm). The phenomenon of self-terminating crystallization at a dimension of 2–5 nm is explained by segregation of Si that is expelled from growing metal carbide grains into the surrounding amorphous phase matrix, which limits diffusion of the metal and carbon.
We report that an electron beam focused for high-resolution imaging rapidly initiates observable crystallization of amorphous Me–Si–C films. For 200-keV electron irradiation of Nb–Si–C and Zr–Si–C films, crystallization is observed at doses of ~2.8 × 109 and ~4.7 × 109 e−/nm2, respectively. The crystallization process is driven by atomic displacement events, rather than heating from the electron beam as in situ annealing (400–600 °C) retains the amorphous state. Our findings demand a critical analysis of alleged amorphous and nanocrystalline ceramics including reassessing previous reports on nanocrystalline Me–Si–C films for possible electron-beam-induced crystallization effects.
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