The efficient utilization of natural resources is critical for conveying society to a more sustainable future. Recently, the Cu-Fe nanocomposites are found to be efficient catalysts for profitable use of biomass- and syngas-based products [1-4], and they are considered as ecofriendly and low-cost altenative to the precious metal catalysts. The method of preparation of the Cu-Fe nanocomposite influences its reducibility and the interaction between Cu and Fe components that can result in wide variation of catalytic properties. In this work, we studied the Cu-Fe nanocomposites prepared by two novel procedures: (i) co-deposition of Cu and Fe precursors on the outer surface of the silica support powder using urea and (ii) deposition of Cu and Fe precursors by consecutive incipient wetness impregnation of porous silica beads with ammonium trioxalatoferrate and copper (II) nitrate solutions. The TGDTA studies showed that the supported precursors decomposed at 300-350 ºC. Interaction of Fe and Cu precursors during preparation has been revealed, which results in the formation of bimetallic oxide nanoparticles after thermal decomposition of deposited precursors. The XRD and TEM analysis confirmed a high dispersion of mono and bimetallic nanoparticles on the SiO2 support. The method of temperature programmed reduction with hydrogen (TPR-H2) was applied to compare the Cu-Fe interaction. The samples were reduced both after deposition and after thermal decomposition of precursors. The TPR-H2 studies included (i) TPR-H2 up to 500°C followed by reduction at this temperature; (ii) in situ reoxidation with oxygen at room temperature and (iii) TPR-H2 of reoxidized sample. The extent of interaction strongly depends on the preparation procedure that affected the catalytic properties of the prepared materials in the reactions of hydrogenation terminal alkynes and nitroarenes with molecular hydrogen.