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The process of intermetallic layers formation in laminated Ni-Al composite has been investigated. Laminated composite consisting of alternating Ni and Al layers was fabricated by the method of vacuum casting. Ni2Al3 and NiAl3 intermetallic compounds were formed on the Ni-Al interface as a result of subsequent heat treatment. Ni2Al3 phase is presented as a continuous layer, intermetallic NiAl3 exists in eutectic composition with aluminum and as the precipitates of complex shape, which grew deep into the aluminum layer. The amount of NiAl3 increases when the diffusion occurs in a liquid state (e.g. when the heat treatment temperature was about 720 °C). Optical and SEM microscopy examinations show that Ni2Al3 phase has a grain structure, the grain size of Ni2Al3 decreases closer to the nickel layer. The lower was the annealing temperature the smaller was Ni2Al3 grain size. Intermetallic layers thickness is directly related to the duration and temperature of annealing.