Synthesis of Non-Cubic Nitride Phases of Va-Group Metals (V, Nb, and Ta) from Metal Powders in Stream of NH3 Gas under Concentrated Solar Radiation

Using a high-flux solar furnace, loosely compacted powders of Va-group transition metal (V, Nb, and Ta) were reacted with stream of NH3 gas (uncracked NH3 gas) being heated by concentrated solar beam to a temperature (T) range between 600 and 1000 °C. From V, sub-nitride V2N (γ phase) and hypo-stoichiometric mono-nitride VN possessing fcc (face-centered cubic) crystal lattice structure (δ phase) were synthesized. On the other hand, in the reaction product from Nb and Ta, hexagonal mono-nitride phase with N/M atom ratio close to 1 (ε phase) was detected. The reaction duration was normalized to be 60 min. In a conventional industrial or laboratory electric furnace, the synthesis of mono-nitride phase with high degree of crystallinity that yield sharp XRD peaks for Va-group metal might take a quite long duration even at T exceeding 1000 °C. In contrast, mono–nitride phase MN of Va-group metal was synthesized for a relatively short duration of 60 min at T lower than 1000 °C being co-existed with lower nitride phases.

Investigation of the nitride phase in a heat-resistant alloy of the Ni – Co – W – Ti system, hardened by internal nitration

In a high-temperature alloy of the Ni – Co – Cr – W – Ti system grade VZh171, using X-ray spectral analysis, scanning and transmission electron microscopy, the composition of the particles of the hardening phase — nitrides after internal nitriding and subsequent heat treatment was studied. It was found that the particles differ on it chemical composition: the main constituent element, titanium or chromium, is proportionally replaced by other alloy components. The nitride compositions near the surface and in the center of the sample differ in the titanium to chromium ratio. After annealing, this difference is smaller, and the chromium content also decreases. It was found that the nitrides formed during nitriding are compounds in which the main forming element, titanium or chromium, is proportionally replaced by other alloy components. The nitride compositions near the surface and in the center of the sample differ in the titanium to chromium ratio. After annealing, this difference is smaller, and the chromium content also decreases.

Extremely hard and tough high entropy nitride ceramics

Simultaneously hard and tough nitride ceramics open new venues for a variety of advanced applications. To produce such materials, attention is focused on the development of high-entropy ceramics, containing four or more metallic components distributed homogeneously in the metallic sublattice. While the fabrication of bulk high-entropy carbides and borides is well established, high-entropy nitrides have only been produced as thin films. Herein, we report on a newel three-step process to fabricate bulk high-entropy nitrides. The high-entropy nitride phase was obtained by exothermic combustion of mechanically-activated nanostructured metallic precursors in nitrogen and consolidated by spark plasma sintering. The fabricated bulk high-entropy nitride (Hf0.2Nb0.2Ta0.2Ti0.2Zr0.2)N demonstrates outstanding hardness (up to 33 GPa) and fracture toughness (up to 5.2 MPa∙m1/2), significantly surpassing expected values from mixture rules, as well as all other reported binary and high-entropy ceramics and can be used for super-hard coatings, structural materials, optics, and others. The obtained results illustrate the scalable method to produce bulk high-entropy nitrides with the new benchmark properties.

Modelling of structure forming in structural steels

The study showed that the influence of alloying elements on the secondary structure formation of the steels containing from 0.19 to 0.37 wt. % carbon; 0.82-1.82 silicon; 0.63-3.03 manganese; 1.01-3.09 chromium; 0.005-0.031 nitrogen; up to 0.25 wt.% vanadium and austenite grain size is determined by their change in the content of vanadium nitride phase in austenite, its alloying and overheating above tac3, and the dispersion of ferrite-pearlite, martensitic and bainitic structures is determined by austenite grain size and thermal kinetic parameters of phase transformations. Analytical dependencies are defined that describe the experimental data with a probability of 95% and an error of 10% to 18%. An analysis results of studying the structure formation of structural steel during tempering after quenching show that the dispersion and uniformity of the distribution of carbide and nitride phases in ferrite is controlled at complete austenite homogenization by diffusion mobility and the solubility limit of carbon and nitrogen in ferrite, and secondary phase quantity in case of the secondary phase presence in austenite more than 0.04 wt. %. Equations was obtained which, with a probability of 95% and an error of 0.7 to 2.6%, describe the real process.

The Effect of the Metal Phase on the Compressive and Tensile Stresses Reduction in the Superhard Nitride Coatings

The influence of the compressive and tensile stresses forming in the nanostructured Ti–Al–N coatings during deposition on their physical-mechanical properties was studied. The modifying influence of metal components (Ni and Cu) introduction into Ti–Al–N coatings, which do not interact with nitrogen and have limited solubility with the nitride phase, was also under research. Coatings were deposited on WC–(6 wt.%)Co carbide cutting inserts with an arc-PVD method using a cathodic vacuum arc evaporation apparatus. The introduction of Ni and Cu to the composition leads to the reduction of nitride phases grain size in both investigated coatings from 120 to 10–12 nm for Ti–Al–Cu–N and to 15–18 nm for Ti–Al–Ni–N. Thus, the hardness increases from 29 to 43 and 51 GPa for the mentioned above coatings, respectively. Meanwhile, Ti–Al–Cu–N and Ti–Al–Ni–N coatings are characterized by tensile stresses about 0.12–0.32 MPa against the much higher value of compressive stresses in Ti–Al–N coatings (4.29–5.31 GPa). The modification of Ti–Al–N coatings also leads to the changing of their destruction mechanism during the scratch-test. The critical loads characterizing the emergence of the first cracks in the coatings and complete abrasion of the coating (Lc1 and Lc3) were determined. They had the value of 20; 22 N (Lc1) and 64; 57 N (Lc3) for Ti–Al–Ni–N; Ti–Al–Cu–N coatings, respectively. The Lc1 parameter for Ti–Al–N coatings was much lower and was equal to 11 N. Along with those, Ti–Al–N coatings destructed according to the adhesion mechanism when the critical load was 35 N. In addition, the decreasing level of compressive stresses in Ti–Al–Cu–N and Ti–Al–Ni–N coatings as compared to that in the Ti–Al–N coating, their crack resistance during multi-cycle shock-dynamic impact test was significantly higher. The results can indicate that high hardness and crack resistance of the coatings is to a greater extent determined by coatings nanostructuring, not the stresses value. In addition, it confirms the possibility to obtain coatings with low stresses value while maintaining their superhardness.

Failure Evaluation of a SiC/SiC Ceramic Matrix Composite During In-Situ Loading Using Micro X-ray Computed Tomography

In this study, we have examined ceramic matrix composites with silicon carbide fibers in a melt-infiltrated silicon carbide matrix (SiC/SiC). We subjected samples to tensile loads while collecting micro X-ray computed tomography images. The results showed the expected crack slowing mechanisms and lower resistance to crack propagation where the fibers ran parallel and perpendicular to the applied load respectively. Cracking was shown to initiate not only from the surface but also from silicon inclusions. Post heat-treated samples showed longer fiber pull-out than the pristine samples, which was incompatible with previously proposed mechanisms. Evidence for oxidation was identified and new mechanisms based on oxidation or an oxidation assisted boron nitride phase transformation was therefore proposed to explain the long pull-out. The role of oxidation emphasizes the necessity of applying oxidation resistant coatings on SiC/SiC.