This study demonstrates the successful synthesis of Ni/Y2O3 nanocomposite particles through the application of ultrasound-assisted precipitation using the Ultrasonic Spray Pyrolysis technique. The particle size was predicted accurately using a modified equation, and they were collected in a water suspension with Polyvinylpyrrolidone (PVP) as the stabiliser. The presence of the Y2O3 core and Ni shell was confirmed with Transmission Electron Microscopy (TEM) and with electron diffraction. The TEM observations revealed the formation of round particles with an average diameter of 466 nm, while the lattice parameter on the Ni particle’s surface was measured to be 0.343 nm. The Ni/Y2O3 nanocomposite particle suspensions were lyophilized, to obtain a dried material that was suitable for embedding into a Polylactic acid (PLA) matrix. The resulting PLA/Ni/Y2O3 composite material was successfully extruded successfully, so that a 3D printed technology Fused Filament Fabrication could be used further for the production of tensile test tubes. The tensile tests showed that the addition of lyophilised Ni/Y2O3 into the PLA matrix decreased the tensile strength by 21.8 %, while the tensile modulus was not influenced. Dynamic Mechanical Analysis (DMA) showed that the addition of the Ni/Y2O3 particles increased the glass transition temperature by 5 °C, and increased the storage modulus in the glass transition range significantly. These findings demonstrate the potential for utilising Ni/Y2O3 nanocomposite particles in 3D printing applications, and warrant further exploration of their mechanical properties and potential applications in various fields.