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The formation and stability of nanoscaled microstructures upon annealing of two amorphous systems have been investigated by small-angle neutron scattering (SANS). The bulk amorphous alloy Zr41Be22.5Ti14Cu12.5Ni10 decomposes into two supercooled liquid phases upon annealing above the glass temperature. Dynamic scaling has been demonstrated for this phase-separation process. Crystallization is significantly slowed down by the two-phase nanoscaled microstructure formed upon decomposition. The temperature and magnetic field dependence of the anisotropic SANS scattering profiles in Fe73.5Si15.5B7M4 (M = Nb, W, Cu) alloys revealed superparamagnetic behaviour of Fe3Si nanocrystals which are decoupled from the amorphous ferromagnetic matrix. An Nb-enriched nonmagnetic layer formed around the Fe3Si crystals during diffusion-limited growth prevents magnetic exchange interactions and the coarsening of the nanocrystals.

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