• Journal of Powder Materials
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• v.11 no.4
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• pp.294-300
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• 2004

This study for preparation of aluminum nitride (AlN) with high purity was carried out by self-propagating high-temperature synthesis method in two different systems, $Al-N_{2}$ and $Al-N_{2}$-AlN, with the change of nitrogen gas pressure and dilution factor. On the occasion of $Al-N_{2}$ system, unreacted aluminum was detected in the product in spite of high nitrogen pressure, 10 MPa, This may be caused by obstructing nitrogen gas flow to inner part of molten and agglomerate of aluminum, formed in pre-heating zone. In $Al-N_{2}$-AlN system, AlN with a purity of 95% or ever can be prepared in the condition of $f_{Dil}\geq0.5$, $P_{N_{2}}\geq$ 1 MPa, and the purity can be elevated to 98% over in the condition of $f_{Dil}$ = 0.7 and $P_{N_{2}}$ = 10 MPa.

• Journal of the Korean Society for Heat Treatment
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• v.18 no.5
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• pp.281-287
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• 2005

Titanium aluminium nitride((TiAl)N) film is anticipated as an advanced coating film with wear resistance used for drills, bites etc. and with corrosion resistance at a high temperature. In this study, (TiAl)N thin films were deposited both at room temperature and at elevated substrate temperatures of 573 to 773 K by using a two-facing-targets type DC sputtering system in a mixture Ar and $N_2$ gases. Atomic compositions of the binary Ti-Al alloy target is Al-rich (25Ti-75Al (atm%)). Process parameters such as precursor volume %, substrate temperature and Ar/$N_2$ gas ratio were optimized. The crystallization processes and phase transformations of (TiAl)N thin films were investigated by X-ray diffraction, field-emission scanning electron microscopy. The microhardness of (TiAl)N thin films were measured by a dynamic hardness tester. The films obtained with Ar/$N_2$ gas ratio of 1:3 and at 673 K substrate temperature showed the highest microhardness of $H_v$ 810. The crystallized and phase transformations of (TiAl)N thin films were $Ti_2AlN+AlN{\rightarrow}TiN+AlN$ for Ar/$N_2$ gas ratio of 1:3, $Ti_2AlN+AlN{\rightarrow}TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 1:1 and $TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN{\rightarrow}Ti_2AlN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 3:1. The above results are discussed in terms of crystallized phases and microhardness.

• Journal of the Korean Ceramic Society
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• v.26 no.1
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• pp.31-36
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• 1989

In order to synthesize AlN-polytypes from AlN-SiO2-Al2O3 system, composition A (AlN/SiO2/Al2O3=1/0.3/0.05, mole ratio) and composition B(AlN-SiO2-Al2O3=1/0.2/0.05, mole ratio) were used. AlN-polytypes were produced by nitriding the mixture at 175$0^{\circ}C$~190$0^{\circ}C$ under N2 atmosphere. For lower reaction temperature, 15R phase was produced and in the case of higher reaction temperature, AlN phase was only produced. As each composition was heated at 185$0^{\circ}C$ in N2 atmosphere, produced main phases were 15R phase for composition A and 21R phase for composition B respectively. The fracture surfaces of produced reactants showed porous skeleton structure.

• Journal of the Korean institute of surface engineering
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• v.36 no.2
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• pp.109-115
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• 2003

Quaternary Ti-Al-Si-N films were deposited on WC-Co substrates by a hybrid deposition system of arc ion plating (AIP) method for Ti-Al source and DC magnetron sputtering technique for Si incorporation. The synthesized Ti-Al-Si-N films were revealed to be composites of solid-solution (Ti, Al, Si)N crystallites and amorphous Si3N4 by instrumental analyses. The Si addition in Ti-Al-N films affected the refinement and uniform distribution of crystallites by percolation phenomenon of amorphous silicon nitride, similarly to Si effect in TiN film. As the Si content increased up to about 9 at.%, the hardness of Ti-Al-N film steeply increased from 30 GPa to about 50 GPa. The highest microhardness value (~50 GPa) was obtained from the Ti-Al-Si-N film haying the Si content of 9 at.%, the microstructure of which was characterized by a nanocomposite of nc-(Ti,Al,Si) N/a$-Si_3$$N_4$.

• Journal of the Korean Society for Heat Treatment
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• v.23 no.2
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• pp.69-74
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• 2010

AlN thin films were deposited by using a two-facing-targets type sputtering system (TFTS), and their deposition characteristics, microstructure and texture were investigated. Total gas pressure was kept constant at 0.4 Pa and the partial pressures of nitrogen, $PN_2$ (($N_2$ pressure)/($Ar+N_2$ pressure)) varied from 0 to 0.4 Pa. The texture of the film cross-sections and surface morphology were observed by field emission scanning electron microscope (FE-SEM). The crystallographic orientation of the films were analyzed by X-ray diffraction (XRD). Deposition of AlN film depends on $N_2$ partial pressure. The best preferred oriented AlN thin films can be deposited at a nitrogen partial pressure of $PN_2$ = 0.52. As-deposited AlN films show preferred orientation and columnar structure, and the grAlN size of AlN films increases with increasing sputtering current.

• Journal of the Korean Ceramic Society
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• v.51 no.5
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• pp.498-504
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• 2014

Particulate nitride composites have been fabricated by sintering the compacted powder of AlN and 5 - 64.3 mol% $Al_2O_3$, with a small addition of $Y_2O_3$ ($Y_2O_3$/AlN, 1 wt%), in 1-atm nitrogen gas at $1650-1900^{\circ}C$. The composites were characterized in terms of sintering behavior, phase relations, microstructure and thermal shock resistance. AlN, 27R AlN pseudopolytype, and alminium oxynitride (AlON, $5AlN{\cdot}9Al_2O_3$) were found to existin the sintered material. Regardless of batch composition, the AlN-$Al_2O_3$ powder compacts exhibited similar sintering behavior; however, the degree of shrinkage commonly increased with increasing $Al_2O_3$ content, consequently giving high sintered bulk density. By increasing the $Al_2O_3$ addition up to ${\geq}50 mol%$, the matrix phase in the sintered material was converted from AlN or 27R to AlON. Above $1850^{\circ}C$, a liquid phase was formed by the reaction of $Al_2O_3$ with AlN, aided by $Y_2O_3$ and mainly existed at the grain boundaries of AlON. Thermal shock resistance was superior in the sintered composite consisting of AlON with dispersed AlN or AlN matrix phase.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.14 no.12
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• pp.972-978
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• 2001

Some effects of Al/N ratio on microstructure of AlN films grown on Si(111) substrates by PAMBE were investigated. Al/N ratio was controlled by rf power of N$_2$ plasma source system. Al excess or N excess conditions were obtained below or above 350 W rf power, respectively. Surface roughness and morphology of AlN film grown at Al/N=1.0 showed the best result. Under Al excess condition, it was suggested that excess Al atoms which did not contribute to the growth of AlN film prevent the normal crystal growth and make abnormal growth of some columns. However, under N excess condition, it was explained that some of the excess active N source turned into gas state and then desorbed out from substrate.

• Journal of the Korean Society for Heat Treatment
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• v.10 no.2
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• pp.138-149
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• 1997

TiN and AlN are ceramic materials with extensive applications due to its excellent mechanical and chemical properties at elevated temperature. The purpose of this research is to develop the method for the synthesis of ternary nitride powder, titanium-aluminum-nitrogen system, which have an excellent property of both TiN and AlN. The ternary nitride such as $Ti_3AlN$, $Ti_2AlN$ and $Ti_3Al_2N_2$ can be synthesized by the interdiffusion nitriding method in Ar gas, however, the ternary nitride coexist with TiN, AlN, $Ti_3Al$ and ${\alpha}$-Ti. The ternary nitride are stable below $1400^{\circ}C$, but these are gradually decomposed into TiN, $Ti_3Al$ and AlN above $1400^{\circ}C$. The thermal oxidation characteristics of the Ti-Al-N compound synthesized by the interdiffusion nitriding method is superior to that of the TiN+AlN mixed powder, and the oxidation for both materials show the differential behaviors.

• Journal of the Korean Ceramic Society
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• v.26 no.1
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• pp.100-108
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• 1989

Aluminum hydroxides were prepared by the alkoxide hydrolysis method using Al-isopropoxide as a starting material and NH4OH as a catalytic agent. When Al-isopropoxide was hydrolyzed in a H2O-NH3 system, only Al(OH)3 was obtained over all pH values. However, AlOOH was formed besides Al(OH)3 when Al-isopropoxide was hydrolyzed in a H2O-NH3-isopropyl alcohol system. The AlOOH/Al(OH)3 ratio was increased as the isopropyl alcohol content was increased. The hydroxides, Al(OH)3 and AlOOH, obtained in this study and the commerical products, $\alpha$-Al2O3 and AlOOH were subjected to the carbothermal reduction and nitridation reaction to product AlN powder, using carbon black as a reducing agent under N2 atmosphere at various temperatures. AlN was synthesized from the obtained Al(OH)3 and the commercial AlOOH at 145$0^{\circ}C$, however, synthesized from the obtained AlOOH and the commercial alpha-alumina at 135$0^{\circ}C$. The temperature difference is assumed to be attributed to the reactivity of those powders. AlN powder prepared from the Al-isopropoxide was observed to have the narrower particle size distribution than that prepared from the commercial $\alpha$-Al2O3 or AlOOH.

• Journal of the Korean Ceramic Society
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• v.24 no.1
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• pp.23-32
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• 1987

Synthesis of high purity ultrafine Si3N4 and ${\beta}$-Sialon powders was investigated via the simultaneous reduction and nitriding of amorphous SiO2, SiO2-Al2O3 system prepaerd by hydrolysis of alkoxides, using carbonablack as a reducing agent. In Si(OC2H5)4-C2H5 OH-H2 O-NH4OH system, hydrolysis rate increased with increasing reaction temperature and pH. Pure ${\alpha}$-Si3N4 was formed at 1350$^{\circ}C$ for 5 hrs in N2 atmosphere. In Si(OC2H5)4-Al(OC3H7)3-C6H6-H2 O-NH4OH system, weight loss increased as Si/Al ratio decreased. Single phase ${\beta}$-Sialon consisted of Si/Al=2 was formed at 1350$^{\circ}C$ in N2 and minor phases of ${\alpha}$-Si3N4, AIN, and X-phase were existed besides theSialon phase at other Si/Al ratios. The Si3N4 and Sialon powders synthesized from alkoxides consisted of uniform find particles of 0.05-0.2$\mu\textrm{m}$ in diameter, respectively.