Due to promising mechanical and chemical properties, transition metal borides have attracted attention, and numerous studies have investigated various combinations of transition elements in hopes of acquiring a final product with desired properties combined. In this study, novel low-temperature approach was adopted for the synthesis of cobalt-titanium-boron based crystalline powders. The method was based on the single-step direct reaction of CoCl2(s), TiCl4(l) and NaBH4(s) in a sealed reactor under autogenic pressure. After the reaction of the precursors at 850 degrees C by using the molar ratios of metal chlorides to NaBH4 as 1:3, CoB and TiB2 phases were formed in-situ. The subsequent annealing process at 1100 degrees C achieved a full conversion of metal chlorides to CoB-TiB2 composite nanostructures. It was concluded that the binary forms of the borides tend to form as separate phases, which is illustrated in the SEM/EDS analyses with different morphologies. Amorphous boron layer surrounded TiB2 particles with an average particle size of 60 nm, whereas the CoB particles formed agglomerates with an average size of 450 nm. The use of synthesized composite powders as reinforcement in metal matrices resulted in enhanced hardness (506 HV) and compressive strength (1682 MPa) of the Ti6Al4V bulk samples. (C) 2020 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.