Synthesis Of Titanium Nitride Research Articles

Titanium Nitride Synthesis during Double Mechanical Activation of Titanium—in Argon and in Nitrogen

Titanium Nitride Synthesis during Double Mechanical Activation of Titanium—in Argon and in Nitrogen

SCRATCH TESTING OF ZrN COATING ON TI-6AL-4V TITANIUM ALLOY SURFACE PRELIMINARY TREATED BY COMPRESSION PLASMA FLOWS IMPACT

Investigation of compression plasma flows preliminary impact influence on adhesion of ZrN coating deposited on Ti-6Al-4V titanium alloy was carried out. Profilometry, X-ray diffraction, and scratchtesting were used as investigation techniques. The findings showed that preliminary plasma impact led to the formation of developed surface relief and synthesis of titanium nitride on the surface of the alloy. Plasma processing provided a higher critical force Lc3 during scratch tests, which increases from 44 N (without processing) to 137 N (the density of absorbed energy 26 J/cm<sup>2</sup>, 6 pulses). With a decrease in the density of absorbed energy and a growth of the number of pulses, there was a tendency of the critical force Lc3 increase, that is mainly associated with the formation of an intermediate layer δ-TiN during plasma impact, the thickness of which increased with a growth of the number of pulses and a decrease in the density of absorbed energy.

Room-Temperature Synthesis of Titanium Nitride Using Metastable Nitrogen

The room-temperature synthesis of titanium nitride (TiN) is presented using the reaction of metastable nitrogen (MSN) with a titanium metal surface. The MSN is generated in a nitrogen glow discharge with plasma-ion filtering using a commercial direct analysis in real time (DART) source. The MSN is flowed over a titanium substrate at ambient pressure producing TiN surfaces that are ultra-clean and suitable for plasmonic applications. This is demonstrated using surface-enhanced infrared absorption spectroscopy (SEIRA), producing a 100-fold signal enhancement. Nitriding using MSN could find general applications in producing nitrided surfaces with small-scale structures.

Discrete One-Stage Mechanochemical Synthesis of Titanium-Nitride in a High-Energy Mill

Discrete (discontinuous) mechanochemical synthesis of titanium nitride was experimentally investigated. The experimental results show that mechanical activation intensifies the chemical conversion in the Ti-N system, and the discrete synthesis of the final product is conducted under “soft” controlled conditions without high heat release. The new theory of mechanochemical synthesis and the mathematical model based on it were used for theoretical evaluation of the dynamics of titanium activation in the nitrogen medium. It was found that the discrete mode of synthesis includes two factors accelerating mechanochemical reactions in the Ti-N synthesis: structural (grinding of metallic reagent and formation of interfacial areas) and kinetic (accumulation of excess energy stored in the formed structural defects in metallic reagent). The kinetic constants of the process were found using experimental data and the inverse problem method. The diagrams defining the controlled modes of obtaining titanium nitride particles with the given characteristics were constructed. A mathematical model for theoretical estimation of the dynamics of activation of titanium powder in the nitrogen medium was developed using a new macrokinetic theory of mechanochemical synthesis.

Synthesis of titanium nitride via hybrid nanocomposites based on mesoporous TiO2/acrylonitrile

In the present study, the synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored. The choice of hybrid nanocomposite as precursor for the synthesis of TiN was made due to the possibility of having an intimate interface between the organic and inorganic phases in the mixture that can favours CRN reaction. Subsequently, the hybrid composites have been subjected to four-step thermal treatments at 290 °C, 550 °C, 1000 °C and 1400 °C under nitrogen atmosphere. The XRD results after thermal treatment at 1000 °C under nitrogen flow show the coexistence of two crystalline phases of TiO2, i.e. anatase and rutile, as well as TiN phase, together with the detection of amorphous carbon that proved the initiation of CRN reaction. Furthermore, the observations based on XRD patterns of samples thermally treated at 1400 °C in nitrogen atmosphere were in agreement with SEM analysis, that shows the formation of TiN by CRN reaction via hybrid nanocomposites mesoporous TiO2/acrylonitrile.

An adept approach to convert titanium carbide to titanium nitride and it’s composite with N-doped carbon nanotubes for efficient oxygen electroreduction kinetics

We report an in situ synthesis of titanium nitride (Ti3N2Tx) from its carbide (Ti3C2Tx) and concurrently composite formation with N-doped carbon nanotubes (N-CNTs). Unlike conventional wet-chemical method, a simple approach has been adopted for the synthesis of Ti3N2Tx and it’s composite with N-CNTs. The crystallographic study shows an obvious phase transformation from carbide to nitride. Importantly, an optimized composite electrocatalyst (Ti3N2@NCNT(20)-800) exhibits promising oxygen reduction ability under alkaline conditions with positive onset potential (Eonset) of 1.0 V versus reversible hydrogen electrode (RHE) and current density (JL) of 5.3 mA/cm2. The remarkable oxygen reduction reaction (ORR) properties mainly originate from the fascinating carbon-nitrogen exchange (Ti3C2Tx into Ti3N2Tx) in the MXene lattice along with N-doping in CNTs, which eventually lead to the formation of their composite and generating enough active centres for dioxygen adsorption followed by electroreduction. Moreover, the rotating ring disk electrode (RRDE) studies were carried to particularly detect peroxide (HO2−) formation and further to get an insight into ORR kinetics. Additionally, a robust performance of Ti3N2@NCNT(20)-800 electrocatalyst over Pt/C has been observed during the electrochemical cycling stability up to 10,000 (10 k) durable cycles. Thus, we believe that the present methodology provides an adept approach to convert carbide into nitride and further to extend it to synthesize the MXene based composite materials for energy conversion applications.

Robust TiN nanoparticles polysulfide anchor for Li–S storage and diffusion pathways using first principle calculations

Abstract Recently, lithium–sulfur (LiS) batteries achieve incredible research interest owing to outstanding theoretical storage capacity, abundant resources, economical, and ecological affability. Nonetheless, the real usage of LS battery obstructs by shuttling-effect of soluble lithium-based polysulfides (LiPSs) that result in languid redox reactions, while the vital diffusion and migration mechanism of Li and S onto TiN surface is yet a myth. Herein, rational synthesis of titanium nitride (TiN) nanoparticles and sulfur composite (TiN-NPs@S) via dry freezing method as cathode material is explored for high efficiency LiS batteries. The ultra-small nanoparticles exhibits high surface area with narrow pores which serve as conductive channels for proficient passage for ions/electrons exchange during electrochemical energy storage reactions. The density functional theory (DFT) computational results, charge density distribution and charge transfer and analysis of geometry constructions indicate TiN surface possess stronger adsorption strength to S atom than Li atom implies TiN as polysulfide adsorbent. The TiN cathode after 100 cycles exhibits an excellent initial capacity of 1279 mAh g−1 at 0.5 C about 75.8% of theoretical capacity (1562 mAh g−1). The hot-to-cold-synthesis method projects formation of ultra-small sized nanoparticles which illuminates bright panorama for Li–S batteries to achieve excellent conductivity, high power density and energy density, which is of great advantageous for industrial applications.

Features of mechanochemical synthesis in the system of solid reagent – active gas

Different modes of mechanochemical synthesis of titanium nitride are found based on the developed mathematical model and experimental data. Approximate analytical formulas are obtained for estimating the characteristics of mechanochemical synthesis during its different stages.

Application of a vacuum-arc discharge for the production of biocompatible coatings

Vacuum-arc discharge is an effective method of forming pure metal and metal-like coatings of complex composition. In this paper, the possibility of its use for the production of biocompatible coatings on the example of synthesis of titanium nitride and titanium carbide on metal substrates is evaluated.

Formation of Biomedical Coatings with Complex Compositions Using Vacuum Arc Plasma

One of the most promising methods for biomedical coating formation is based on the use of vacuum arc plasma sources that allow pure metals to be obtained and plasma-chemical synthesis of complex compounds to be carried out. In this work, the results of synthesis of titanium nitride and titanium carbide on metal substrates using specially developed equipment are presented.

Self-propagating high-temperature synthesis of titanium nitride with the participation of ammonium chloride

We have studied the combustion of titanium in nitrogen in the presence of ammonium chloride. It has been shown that the use of NH4Cl in the self-propagating high-temperature synthesis of TiN considerably reduces the combustion temperature, prevents sintering of the synthesized titanium nitride particles, and increases their specific surface area. The synthesis products have the form of nanostructured titanium nitride particles which reproduce the shape of the starting titanium particles but consist of equiaxed titanium nitride grains ranging in size from 50 to 500 nm. We have obtained nanostructured titanium nitride powders ranging in specific surface area up to 80 m2/g.

Titanium nitride plasma-chemical synthesis with titanium tetrachloride raw material in the DC plasma-arc reactor

The possibility of plasmochemical synthesis of titanium nitride is demonstrated in the paper. Results of the thermodynamic analysis of TiCl4 – H2 – N2 system are presented; key parameters of TiN synthesis process are calculated. The influence of parameters of plasma-chemical titanium nitride synthesis process in the reactor with an arc plasmatron on characteristics on the produced powders is experimentally investigated. Structure, chemical composition and morphology dependencies on plasma jet enthalpy, stoichiometric excess of hydrogen and nitrogen in a plasma jet are determined.

Synthesis of titanium nitride and carbonitride nanopowders in confined-jet flow plasma reactor

The synthesis of titanium nitride and carbonitride nanopowders from titanium tetrachloride vapor in a stream of hydrogen–nitrogen plasma, generated by an arc torch, in confined-jet flow reactor has been experimentally studied. Single-phase nanopowders with a NaCl-type cubic crystal lattice as assemblies of preferably cube-shaped nanoparticles of a 20–150 nm size and aggregates based on them have been obtained in the experiments. By varying the synthesis parameters, it has been possible to prepare titanium nitride nanopowders with a specific surface area in the range of 11–39 m2/g containing 18.8–22.5 wt % nitrogen, which corresponds to the empirical formula TiN0.79–TiN0.99. The titanium carbonitride nanopowders had a specific surface area of 13–23 m2/g and carbon and nitrogen contents of 7.5–13.6 and 13.5–5.1 wt %, respectively.

Equilibrium energy and technological characteristics of plasma synthesis of titanium nitride, carbide, and carbonitride from titanium tetrachloride

Equilibrium energy and technological characteristics of the plasma synthesis of titanium nitride, carbide, and carbonitride, in particular, the composition and yields of final products, energy consumption upon their production, and the required enthalpy of a plasma flow, are calculated for the following reactions: TiCl4 + xH2 + yN2 (synthesis of TiN), TiCl4 + xH2 + zC m H n (synthesis of TiC), and TiCl4 + xH2 + y 1N2 + z 1C m H n (synthesis of TiCN). The calculations are carried out for the temperature range from 500 to 4000 K, at the total pressure of 0.1 MPa in the system, and with the following molar ratios of reagents: x = 8, x = 20; y = 0.5, y = 5, y = 20; z = 0.9, z = 1.0, z = 1.1; y 1 = 5; z 1 = 0.4, z 1 = 0.5, z 1 = 0.6.

Periodic oxidation for fabricating titanium oxynitride thin films via atomic layer deposition

This paper demonstrates thermal atomic layer deposition (ALD) combined with periodic oxidation for synthesizing titanium oxynitride (TiON) thin films. The process used a typical ALD reactor for the synthesis of titanium nitride (TiN) films wherein oxygen was supplied periodically between the ALD-TiN cycles. The great advantage of the process proposed here was that it allowed the TiN films to be oxidized efficiently. Also, a uniform depth profile of the oxygen concentration in the films could be obtained by tuning the oxidation conditions, allowing the process to produce a wide variety of TiON films. The resistivity measurement is a convenient method to confirm the reproducibility of metal film fabrication but may not be applicable for TiON films depending upon the oxidation condition because the films can easily turn into insulators when subjected to periodic oxidation. Therefore, an alternative reproducibility confirmation method was required. In this study, spectroscopic ellipsometry was applied to monitor the variation of TiON films and was able to detect changes in film structures such as conductor–insulator transitions in the TiON films.

Titanium Nitride Synthesis in the Presence of Iodine

A method is proposed for synthesizing titanium nitride by nitriding titanium metal powder with nitrogen in the presence of iodine vapor, and results are given for its application. It is shown that iodine significantly reduces the nitriding reaction activation energy. It is established that TiN forms even at 250°C. It is detected that the size of TiN crystal blocks formed depends on temperature. A nitriding mechanism is proposed.

Plasma synthesis of titanium nitride, carbide and carbonitride nanoparticles by means of reactive anodic arc evaporation from solid titanium

Plasma methods using the direct evaporation of a transition metal are well suited for the cost-efficient production of ceramic nanoparticles. In this paper, we report on the development of a simple setup for the production of titanium-ceramics by reactive anodic arc evaporation and the characterization of the aerosol as well as the nanopowder. It is the first report on TiC X N1 − X synthesis in a simple anodic arc plasma. By means of extensive variations of the gas composition, it is shown that the composition of the particles can be tuned from titanium nitride over a titanium carbonitride phase (TiC X N1 − X ) to titanium carbide as proven by XRD data. The composition of the plasma gas especially a very low concentration of hydrocarbons around 0.2 % of the total plasma gas is crucial to tune the composition and to avoid the formation of free carbon. Examination of the particles by HR-TEM shows that the material consists mostly of cubic single crystalline particles with mean sizes between 8 and 27 nm.

Synthesis of titanium nitride for self-aligned gate AlGaN/GaN heterostructure field-effect transistors.

In this study, titanium nitride (TiN) is synthesized using reactive sputtering for a self-aligned gate process. The Schottky barrier height of the TiN on n-GaN is around 0.5 to 0.6 eV and remains virtually constant with varying nitrogen ratios. As compared with the conventional Ni electrode, the TiN electrode presents a lower turn-on voltage, while its reverse leakage current is comparable with that of Ni. The results of annealing evaluation at different temperatures and duration times show that the TiN/W/Au gate stack can withstand the ohmic annealing process at 800°C for 1 or 3 min. Finally, the self-aligned TiN-gated AlGaN/GaN heterostructure field-effect transistors are obtained with good pinch-off characteristics.

Synthesis of titanium nitride by anodic polarization of titanium in electrolytes based on ethylene glycol

Possibility of forming titanium nitride films by anodic polarization in water-containing ethylene glycol in the presence of various electrically conducting additives was demonstrated and substantiated. The electrochemical processes were studied by chronoamperometry and cyclic voltammetry. Titanium nitride films were subjected to microstructural, X-ray diffraction, and elemental analyses.

Synthesis of titanium nitride by anodic polarization of titanium

Possibility of forming titanium nitride by anodic polarization of the surface of titanium in water-containing organic electrolytes in the presence of NH4F at potentials of 2–14 V was demonstrated and substantiated. The method of cyclic voltammetry was used to study electrochemical processes in electrolytes based on ethylene glycol and glycerol. Results obtained in an analysis of the structural, chemical, and physicomechanical properties of the titanium nitride layers obtained in the study are presented.