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Using the method of reductive thermolysis of two-component precursors, a series of microdispersed alloys Ni1–xRux containing up to 10 at % ruthenium was obtained. The effect of ruthenium content in the alloy on its activity in the catalytic pyrolysis of a mixture of C2–C4 hydrocarbons to produce carbon nanofibers (CNF) was studied. Using the Ni0.98Ru0.02 sample as an example, the early stage of carbon erosion, leading to the disintegration of the alloy and to the formation of active particles, was studied in detail. The obtained alloys were used for the synthesis of metal-carbon nanocomposites Ni1–xRux@CNF, which are promising materials for solving applied problems. [ABSTRACT FROM AUTHOR]