This work investigates the effect of titanium content and the duration of mechanical alloying on the structural and phase state of powder mixtures in the Ni–Al–Ti system. The initial mixtures of Ni₆₈Al₂₅Ti₇, Ni₇₂Al₂₂Ti₆, Ni₇₀Al₂₁Ti₉, and Ni₇₅Al₂₅ were subjected to high-energy milling in a planetary ball mill for 1–6 h. It was found that the addition of titanium accelerates the dissolution of components and promotes the formation of a supersaturated fcc Ni(Al,Ti) solid solution. The most pronounced effects were observed for the Ni₇₀Al₂₁Ti₉ composition, where after 6 h of alloying, the minimum crystallite size (11.3 nm) and maximum lattice strain (1.52%) were achieved. It is shown that titanium reduces the tendency for cold welding and promotes more uniform particle refinement. The optimal conditions for synthesizing a nanocrystalline solid solution with a homogeneous structure are a titanium content of 9 at.% and a mechanical alloying duration of 6 h. The resulting powders are promising for subsequent sintering and application in structural and heat-resistant intermetallic alloys and coatings.

Boron nitride is considered a promising material for solid-state hydrogen storage due to its high thermal and chemical stability up to ~1000 °C, depending on the atmosphere, as well as its ability to form defect-rich structures with enhanced sorption activity. Despite the growing interest in modified BN systems, systematic studies on the effect of multicomponent modification induced by the addition of carbon, titanium, and aluminum on the structural and phase evolution of boron nitride during high-energy mechanical alloying remain limited to date. In this work, the structural-phase and morphological changes in boron nitride-based composites modified by the addition of carbon, titanium, and aluminum, synthesized by high-energy mechanical alloying, were investigated. The structural state and morphology of the materials were analyzed using X-ray diffraction, scanning electron microscopy, particle size analysis, and thermal analysis. It is shown that mechanical alloying leads to a progressive breakdown of the layered hexagonal BN structure and the formation of an amorphous-like, defect-rich state without the formation of new crystalline phases. The main stage of amorphization occurs within 30–60 min, after which structural disordering reaches saturation. Increasing the mechanical alloying time to 120 min does not result in significant changes in the phase state; however, it is accompanied by a reduction in agglomeration and the formation of a more homogeneous powder morphology, characterized by narrower particle size distributions, smoother particle surfaces, and more uniform spatial dispersion of components. It was established that the nature of the added component significantly influences the kinetics of structural transformations: carbon accelerates amorphization, titanium intensifies fragmentation and defect accumulation, whereas aluminum exhibits a stabilizing effect. In multicomponent BN–C–Ti–Al systems, a synergistic combination of these effects is observed, leading to the formation of metastable, partially amorphous structures. Based on a comprehensive analysis of structural and morphological data, the optimal mechanical alloying time was determined to be 120 min, providing a saturated amorphous-like structural state combined with improved microstructural homogeneity. The obtained defect-rich boron nitride structures can be considered a promising basis for further studies in the field of solid-state hydrogen storage.