The development of beta titanium alloys with biocompatible elements to replace Al and V is a subject of significant interest in the biomedical industry. This approach aims to enhance biocompatibility and mitigate potential cytotoxic effects associated with traditional alloying elements. In this work, Ti–xNb–ySi alloys were produced using powder metallurgy, with x of 35, 40, and 45 wt.%, and y of 0.10, 0.35, and 0.60% wt.%, using a $3^2$ experimental design. Milling was used to mix and disperse the powders, followed by cold pressing, sintering, and heat treatment. Nb was the main element used to stabilize the β phase, and Si was used to form Si precipitates, although Si also exhibits a β-stabilizing effect. It was found that an increase from 0.10 to 0.35 wt.% of Si improved relative density, with no benefits observed at 0.60 wt.% Si. Electron microscopy showed the presence of β phase grains, and grains with β + α intragranular structures and precipitates. Increasing Nb content resulted in a decrease in ultimate tensile strength while increasing Si content from 0.10% to 0.35 wt.% exhibited the opposite effect.

This work presents a novel method for producing metal matrix nanocomposite powders using an in situ precipitation technique. As a proof‐of‐concept, TiN nanoparticles are synthesized directly on the surface of FeTi intermetallic powder particles (d ₉₀ < 8.0 μm) through plasma‐assisted nitriding treatment. An equipment is specially designed to enable the movement of powder particles under a controlled 33%H ₂ + 67%N ₂ atmosphere in a rotating drum anode placed around a hollow‐cathode discharge producing the nitrogen reactive species. Plasma operating parameters are fixed at −650 V (cathode potential) and 1.5 Torr (gas pressure), and the treatments are carried out at 550 °C for 4 h. Treated particles’ surface analysis indicated the formation of TiN spherical nanoparticles distributed all over the particle. In addition to the TiN phase, the diffractograms showed the formation of the α‐Fe (ferrite). The presence of N in the samples, as well as the chemical bond between Ti and N, is measured by X‐ray photoelectron spectroscopy (XPS) analysis. The results demonstrated the feasibility of producing nitride‐reinforced nanocomposite powders through an in situ technique using a new plasma‐assisted nitriding process for metallic powders. This approach opens up a huge field for the development of other metallic matrix nanocomposites.