This work is devoted to the synthesis of titanium nitroborides by mechanochemical synthesis followed by spark plasma sintering (SPS) and plasma spheroidization. The obtained materials did not meet the requirements of the grain size composition for further plasma spraying and use as wear-resistant sprayed coatings. To consolidate the particles, spray drying of the material was carried out. The absence of the stoichiometric composition of Ti3B2N after 20 hours of mechanical treatment of the TiN – TiB2 mixture indicates that either the time or the energy saturation of the process for synthesis is insufficient. However, if we use metallic titanium (Ti), boron nitride (BN) and titanium diboride (TiB2) instead of the above binary compounds as initial components, the processing time can be reduced to 5 hours: this period already produces a compound with the stoichiometry close to the required one. The range of hardness values for the obtained compounds after SPS is from 16800 to 22560 MPa, 19570 MPa on average.