Influence of ammonia gas exposure on microstructure of nanocrystalline titanium nitride powder synthesized from titanium dioxide

Alhussain, Hanan; Mise, Takuto; Matsuo, Yasuyuki; Kiyono, Hajime; Nishikiori, Kaoru; Akashi, Takaya

doi:10.2109/jcersj2.19129

Cited by 6 publications

(4 citation statements)

References 19 publications

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“…TiN can be efficiently prepared by nitridation of titanium metal powders or titanium chloride with nitrogen/ammonia and by carbothermal reduction-nitridation of various titanium oxygen-bearing precursors. Many of these syntheses have been directed towards thin film nanostructures [ 22 , 23 , 24 ] and nanocrystalline powders [ 25 , 26 , 27 ].…”

Section: Introductionmentioning

confidence: 99%

Composite Nitride Nanoceramics in the System Titanium Nitride (TiN)-Aluminum Nitride (AlN) through High Pressure and High Temperature Sintering of Synthesis-Mixed Nanocrystalline Powders

et al. 2021

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Presented is a study on the original preparation of individual and in situ intimately mixed composite nanocrystalline powders in the titanium nitride-aluminum nitride system, Ti:Al = 1:1 (at.), which were used in high pressure (7.7 GPa) and high temperature (650 and 1200 °C) sintering with no binding additives for diverse individual and composite nanoceramics. First, variations in precursor processing pathways and final nitridation temperatures, 800 and 1100 °C, afforded a pool of mixed in the nanosized regime cubic TiN (c-TiN) and hexagonal AlN (h-AlN) composite nanopowders both with varying average crystallite sizes. Second, the sintering temperatures were selected either to preserve initial powder nanocrystallinity (650 °C was lower than both nitridation temperatures) or promote crystal growth and recrystallization (1200 °C was higher than both nitridation temperatures). Potential equilibration towards bimetallic compounds upon solution mixing of the organometallic precursors to nanopowders, monomeric Ti[N(CH3)2]4 and dimeric {Al[N(CH3)2]3}2, was studied with 1H and 13C NMR in C6D6 solution. The powders and nanoceramics, both of the composites and individual nitrides, were characterized if applicable by powder XRD, FT-IR, SEM/EDX, Vicker’s hardness, and helium density. The Vicker’s hardness tests confirmed many of the composite and individual nanoceramics having high hardnesses comparable with those of the reference h-AlN and c-TiN ceramics. This is despite extended phase segregation and, frequently, closed microsized pore formation linked mainly to the AlN component. No evidence was found for metastable alloying of the two crystallographically different nitrides under the applied synthesis and sintering conditions. The high pressure and high temperature sintering of the individual and in situ synthesis-mixed composite nanopowders of TiN-AlN was demonstrated to yield robust nanoceramics.

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Section: Introductionmentioning

confidence: 99%

Composite Nitride Nanoceramics in the System Titanium Nitride (TiN)-Aluminum Nitride (AlN) through High Pressure and High Temperature Sintering of Synthesis-Mixed Nanocrystalline Powders

et al. 2021

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“…Many of them are semiconductors, and examples include the wide-bandgap semiconductor gallium nitride GaN, E g = 3.4 eV for hexagonal polytype and 3.2 eV for cubic polytype, the narrow-bandgap indium nitride InN, E g = 0.7–0.8 eV, and their intermediate-bandgap binary solid solutions of In x Ga 1−x N with E g = 0.7–3.4 eV and Al x Ga 1−x N with E g = 3.4–6.2 eV [ 5 ]. Additional important materials applications dwell on unique sets of properties all-in-one; for instance, aluminum nitride AlN displays a coexistence of electrical insulating properties with high thermal conductivity [ 6 ], whereas titanium nitride TiN provides an advantageous combination of tough mechanical and thermal resistance with extremely low electrical resistivity [ 7 ]. Other nitride materials that receive considerable attention are boron nitride BN [ 8 ] and silicon nitride Si 3 N 4 [ 9 ].…”

Section: Introductionmentioning

confidence: 99%

New Nitride Nanoceramics from Synthesis-Mixed Nanopowders in the Composite System Gallium Nitride GaN–Titanium Nitride TiN

et al. 2021

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Presented is a study on the preparation, via original precursor solution chemistry, of intimately mixed composite nanocrystalline powders in the system gallium nitride GaN–titanium nitride TiN, atomic ratio Ga/Ti = 1/1, which were subjected to high-pressure (7.7 GPa) and high-temperature (650, 1000, and 1200 °C) sintering with no additives. Potential equilibration toward bimetallic compounds upon mixing of the solutions of the metal dimethylamide precursors, dimeric {Ga[N(CH3)2]3}2 and monomeric Ti[N(CH3)2]4, was studied with 1H- and 13C{H}-NMR spectroscopy in C6D6 solution. The different nitridation temperatures of 800 and 950 °C afforded a pool of in situ synthesis-mixed composite nanopowders of hexagonal h-GaN and cubic c-TiN with varying average crystallite sizes. The applied sintering temperatures were either to prevent temperature-induced recrystallization (650 °C) or promote crystal growth (1000 and 1200 °C) of the initial powders with the high sintering pressure of 7.7 GPa having a detrimental effect on crystal growth. The powders and nanoceramics, both of the composites and of the individual nitrides, were characterized if applicable by powder XRD, SEM/EDX, Raman spectroscopy, Vicker’s hardness, and helium density. No evidence was found for metastable alloying of the two crystallographically different nitrides under the applied synthesis and sintering conditions, while the nitride domain segregation on the micrometer scale was observed on sintering. The Vicker’s hardness tests for many of the composite and individual nanoceramics provided values with high hardness comparable with those of the individual h-GaN and c-TiN ceramics.

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“…They get therefore oxidized (Fig. 11) and diffractions peaks shift to a TiO compound 55,63 . In opposition to tetragonal anatase (PDF 00-021-1272), this compound exhibits a cubic structure like TiN, as well as a close lattice parameter.…”

Section: Crystalline Structurementioning

confidence: 99%

Conductive TiN thin films grown by plasma-enhanced atomic layer deposition: Effects of N-sources and thermal treatments

Badie

Tissot

Sciacca

et al. 2023

Journal of Vacuum Science &Amp; Technology A

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This work consists of optimizing TiN plasma-enhanced atomic layer deposition using two different N-sources: NH[Formula: see text] and N[Formula: see text]. In addition to maximizing the growth per cycle (GPC) and to shorten the deposition duration, comprehensive in situ and ex situ physicochemical characterizations give valuable information about the influence of the N-source nature, their dilution in Ar, and the plasma power on layer’s final properties. N[Formula: see text] and NH[Formula: see text] dilutions within Ar are extensively investigated since they are critical to decreasing the mean free path ([Formula: see text]) of plasma-activated species. A 1:1 gas ratio for the N-sources:Ar mixture associated with low flows (20 sccm) is optimal values for achieving highest GPCs (0.8 Å/cycle). Due to lower reactivity and shorter [Formula: see text] of the excited species, N[Formula: see text] plasma is more sensitive to power and generator-to-sample distance, and this contributes to lower conformality than with NH[Formula: see text] plasma. The resistivity of the initial amorphous films was high ([Formula: see text] cm) and was significantly reduced after thermal treatment ([Formula: see text] cm). This demonstrates clearly the beneficial effect of the crystallinity of the film conductivity. Though N[Formula: see text] process appears slightly slower than the NH[Formula: see text] one, it leads to an acceptable film quality. It should be considered since it is nonharmful, and the process could be further improved by using a reactor exhibiting optimized geometry.

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Influence of ammonia gas exposure on microstructure of nanocrystalline titanium nitride powder synthesized from titanium dioxide

Cited by 6 publications

References 19 publications

Composite Nitride Nanoceramics in the System Titanium Nitride (TiN)-Aluminum Nitride (AlN) through High Pressure and High Temperature Sintering of Synthesis-Mixed Nanocrystalline Powders

Composite Nitride Nanoceramics in the System Titanium Nitride (TiN)-Aluminum Nitride (AlN) through High Pressure and High Temperature Sintering of Synthesis-Mixed Nanocrystalline Powders

New Nitride Nanoceramics from Synthesis-Mixed Nanopowders in the Composite System Gallium Nitride GaN–Titanium Nitride TiN

Conductive TiN thin films grown by plasma-enhanced atomic layer deposition: Effects of N-sources and thermal treatments

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