Synthesis of titanium nitride by a spark-discharge method in liquid ammonia

Sato, Teruyuki; Yasuda, Shigeru; Usuki, Kazuyuki; Yoshioka, Toshiaki; Okuwaki, Akitsugu

doi:10.1007/bf01152967

Cited by 16 publications

(9 citation statements)

References 5 publications

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“…However, only rutile and TiN were observed for the reaction of NH 3 and rutile at 700°C . In summary therefore, it can be concluded from the present and previous studies that the reaction process differs a lot when using different precursors as starting material …”

Section: Resultssupporting

confidence: 58%

“…20 In summary therefore, it can be concluded from the (6) 6TiO 2 + 8NH 3 (g) → 6TiN + 12H 2 O (g) + N 2 (g) ΔG Θ = 914790−726.7T (J/mol) present and previous studies that the reaction process differs a lot when using different precursors as starting material. 20,32,33 In this study, micrometer-sized anatase TiO 2 was used as the starting material. The reaction mechanisms can be described by the schematic presented in Figure 10.…”

Section: Reduction and Nitridation Mechanismsmentioning

confidence: 99%

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Mechanism on reduction and nitridation of micrometer‐sized titania with ammonia gas

et al. 2020

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Ammonia gas can be simultaneously used as a reductant and nitrogen source to prepare TiN from titania. In this work, the mechanisms on reduction and nitridation of micrometer‐sized anatase with ammonia gas have been investigated, using both thermodynamic and experimental studies. The thermodynamic analysis indicated that reduction and nitridation of TiO2 by NH3 was feasible. Anatase will undergo different paths to form TiN, depending on the reaction temperature. Upon heating, NH3 was seen to partially decompose into N2 and H2, although the actual NH3 decomposition ratio was less than the theoretical value. The experimental results indicated that the obtained titanium nitride was non‐stoichiometric (TiNxO1−x, x ≤ 1), as it contained a certain amount of oxygen. Based on the phase transformation and X‐ray photoelectron spectroscopy analysis, the reduction and nitridation routes were deduced: TiO2 reacted with NH3 to form TiNxO1−x directly, at lower temperatures, and followed the path TiO2 → TinO2n−1 → TiNxO1−x, at higher temperatures. TinO2n−1 was determined to be Ti4O7 and Ti3O5 at 1100°C and 1200°C, respectively. Reaction temperature and time significantly affected the oxygen and nitrogen contents in TiNxO1−x, with the lattice parameter of roasted products gradually increasing—approaching those of pure TiN—with an increase in reaction temperature and holding time. At the same time, the content of oxygen in TiNxO1−x decreased, and its nitrogen content correspondingly increased.

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Section: Resultssupporting

confidence: 58%

Section: Reduction and Nitridation Mechanismsmentioning

confidence: 99%

Mechanism on reduction and nitridation of micrometer‐sized titania with ammonia gas

et al. 2020

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“…Nakajima and Shimada 4 investigated the electrochemical synthesis of TiN precursors and their conversion to nanosized particles, including complicated processes of polymerization, heat treatment for post‐processing, and pyrolysis under an ammonia atmosphere at 200°–1000°C in vacuum in order to produce TiN. Sato et al 8 . investigated the synthesis of TiN nano powder using an electrical discharge of titanium metals in liquid ammonia.…”

Section: Introductionmentioning

confidence: 99%

Production of Nanocrystalline Titanium Nitride Powder by Atmospheric Microwave Plasma Torch in Hydrogen/Nitrogen Gas

Shin

Hong

Uhm

2005

Journal of the American Ceramic Society

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Nanocrystalline titanium nitride (TiN) particles were directly synthesized in an atmospheric microwave plasma torch, using gas-phase titanium tetrachloride (TiCl 4 ), with N 2 and H 2 as reactants. The gas-phase TiCl 4 was injected with H 2 gas into the microwave plasma-torch flame generated by N 2 swirl gas, and then the dark blue powders were deposited on the inner wall of the quartz tube. The synthesized powder samples were analyzed by scanning electron microscopy (SEM), SEM-EDX, X-ray diffractometer (XRD), transmission electron microscopy, and FT-Raman. The average crystallite sizes of TiN measured from XRD patterns decreased from 15.5 to 11.6 nm, as the flow rate of H 2 injected into the microwave plasma torch increased from 0.03 to 0.3 liters per minute.

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“…Considering the excited condition of the exploded wire material, it is easy to induce reaction between the dissimilar reactive atoms such as liquid nitrogen. The synthesis of titanium nitride through sparks between titanium electrodes in liquid nitrogen and ammonia has been reported [10,11], respectively. Using self-propagating high-temperature synthesis (SHS), the synthesis of bulk titanium nitride has been investigated by Odawara and co-workers [12][13][14] by igniting titanium powders immersed in liquid nitrogen to have a continuous reaction.…”

Section: Introductionmentioning

confidence: 99%