• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.893-901
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• 1994

In this study, AlN powder of fine particle size and of high purity was synthesized by the carbothermal reduction-nitridation of monodisperse, spherical Al(OH)3 which had been prepared by sol-gel method using Al(O-sec-C4H9)3 as the starting material. Depending on the mixing order and kinds of reducing agents, the optimum condition for the preparation of AlN was determined as follows. AlN single-phase was produced by the carbothermal reduction-nitridation of (1) Benzene-washed Al(OH)3 and the reducing agent, carbon, which was mixed in a ball mill: for 5 hours at 140$0^{\circ}C$ under NH3 atmosphere; (2) The mixture prepared by hydrolysis of alkoxide solution into which carbon had been dispersed beforehand: for 5 hours at 135$0^{\circ}C$ ; (3) Al(OH)3 Poly(furfuryl alcohol) composite powder: for 2.5 hours at 135$0^{\circ}C$; (4) The mixture of Al(OH)3 and polyacrylonitrile: for 5 hours at 140$0^{\circ}C$. Addition of CaF2 increased the nitridation rate when carbon or polyacrylonitrile was used as the reducing agent; but it had no effect on the nitridation rate when furfuryl alcohol was used as the reducing agent.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.5
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• pp.223-228
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• 2017

Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.30 no.7
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• pp.441-446
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• 2017

Aluminum nitride fibers were synthesized by carbothermal reduction and nitridation of precursor fibers obtained by electrospinning. The starting materials used to synthesize the AlN fibers were $Al(NO_3)_3{\cdot}9H_2O$ and urea. Polyvinylpyrrolidone with increasing viscidity was used as the carbon source to obtain a composite solution. The mixed solution was drawn into a plastic syringe with a stainless steel needle, which was used as the spinneret and connected to a 20 kV power supply. A high voltage was supplied to the solution to facilitate the formation of a dense net of fibers on the collector. The precursor fibers were dried at $100^{\circ}C$ and then heated to $1,400^{\circ}C$ for 1 h in a microwave furnace under $N_2$ gas flow for the carbothermal reduction and nitridation. X-ray diffraction studies indicated that the synthesized fibers consisted of the AlN phase. Field emission scanning electron microscopy studies indicated that the diameter of the calcined fibers was approximately 100 nm.

• Journal of the Korean Chemical Society
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• v.32 no.3
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• pp.267-275
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• 1988

Fine powders of amorphous $Al_2O_3,\;SiO_2,\;Al_2O_3-SiO_2$ system were prepared by hydrolysis of solutions containing alkoxides, aluminium tri-isopropoxide and silicon tetra-ethoxide. High purity ultrafine ${\beta}-sialon$ powders were prepared by the carbothermal reduction-nitridation of amorphous $Al_2O_3-SiO_2$ powders mixed with carbon black as a reducing agent. In the hydrolysis step the effect of the factors such as pH, reaction temperature and amount of water on the conversion rate of alkoxides to oxides was investigated. In the carbothermal reduction-nitridation the reaction path was assumed by the analysis of intermediates formed in the process of ${\beta}-sialon$ synthesis and the reaction kinetics of ${\beta}-sialon$ formation was considered.

• Journal of the Semiconductor & Display Technology
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• v.16 no.4
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• pp.11-15
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• 2017

Red phosphors, $Sr_2Si_5N_8:Eu^{2+}$, were synthesized as a single-phase crystal structure by optimizing carbon and $Eu^{2+}$ contents in a carbothermal reduction nitridation method. With increasing $Eu^{2+}$ contents, the photoluminescence spectra were red-shifted from 600 nm peak for 1 mol% for to 700 nm for 7 mol%. It was suggested that this red shift is attributed to the energy transfer from one low-energy sited $Eu^{2+}$ (1) to other high-energy sited $Eu^{2+}$ (2). Finally, the best red sample (620 nm emission peak and 80 nm half width for 3 mole% of $Eu^{2+}$) was packaged on a Blue LED together with two additional green and yellow phosphors, the fabricated White LED showed a high color-rendering index of 90 and white color coordinates of x= 0.321 and y = 0.305.

• Journal of the Korean Ceramic Society
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• v.28 no.6
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• pp.465-470
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• 1991

AlN powder was synthesized by carbothermal reduction and nitridation of aluminum hydroxides precipitated in 5∼11 pH range from Al2(SO4)3$.$18H2O aqueous solution. Nitridation reactivity of hydroxide, which depends on precipitation pH, reaction temperature and time, was examined by XRD analysis at 1200∼1350$^{\circ}C$ and compared with that of commercial ${\alpha}$-Al2O3. Hydroxides obtained at higher pH could be more easily nitridated and, considering DTA/TG and BET results, the reason seems to be specific surface area difference of reactants depending on the content of decomposed structural water and the transition rate from transition-Al2O3 to ${\alpha}$-Al2O3.

• Journal of the Korean Ceramic Society
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• v.39 no.3
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• pp.272-277
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• 2002

Aluminum nitride (AlN) powders and whiskers were synthesized by a modified carbothermal reduction and nitridation where a ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ complex is used as precursor. The AlN powders were obtained by calcining the complex without mixing any carbon source under a flow of nitrogen in the temperature range 1200∼1500$^{\circ}$C and then burning out the residual carbon. The nitridation process was investigated by $^{27}Al$ magic-angle spinning (MAS) unclear magnetic resonance, infrared spectroscopy and X-ray diffraction. The complex is pyrolyzed, converted to ${\rho}$- and ${\gamma}$- alumina and then nitridated to AlN without ${\gamma}-{\alpha}$ alumina transition. The morphology of ${\gamma}$-alumina, when it was converted to AlN, was retained, strongly indicating that ${\gamma}$-alumina is converted to AlN through solid-state $AlO_xN_y$, not through gaseous intermediates such as aluminum and aluminaum suboxides. AlN whiskers were obtained, when a (0001) sapphire was used as a catalyst.

• Journal of the Korean Ceramic Society
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• v.23 no.5
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• pp.17-24
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• 1986

β'-Sialon with different compositions was synthesized by the carbothermal reduction-nitridation of compacts containing kaolin graphite and silicon or aluminum at temperature of 1300-1450℃ under flowing gas of 90% N2-10% H2 or 20hrs. Quantitative analysis of minerals which were formed in the specimens was carried out by using the calibration curve which has been prepared from X-ray diffraction patterns. The obtained results were as follows : 1. In the formation of β'-Sialon by carbothermal reduction-nutridation of Si-Al-O-C system mixtures at 1400℃ for 20hrs. (2) β'-Sialon as a major mineral and α-Al2O3 as a minor mineral were identified in the specimen which was prepared of kaolin and graphite. (3)α-Al2O3 and 15R as a minor minerals were measured in the specimen which was prepared of kaolin aluminum and graphite. (4) AlN instead of α-Al2O3 and 15R was formed in the compacts that excess graphite(=35 wt%) was added to the mixture of kaolin and aluminium. 2. As the reaction time and temperature were increased the formation of β'-Sialon was increased whereas the phases of mllite SiC and Si2ON2 were decreased gradually.

• Journal of the Korean Ceramic Society
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• v.26 no.6
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• pp.771-782
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• 1989

Synthesis of $\beta$-Sialon powder was attempted with carbothermal reduction of porous glass. The porous glass was prepared by heat and hydrothermal treatments of 9.32 Li2O.46.5B2O3.37.2SiO2.6.98Al2O3 glass. Carbon pyrolyzed from propane gas was deposited on the porous glass, thereafter activated carbon was added as reducing agents. The synthesized $\beta$-Sialon powder was pressureless sintered at 175$0^{\circ}C$ for 1hr in N2 atmosphere. The characterization of the $\beta$-Sialon powder was performed with XRD, BET, SEM and particle size analysis. The sinterability and mechanical properties of the sintered bodies were investigated in terms of bulk density, M.O.R., fracture toughness, morphology of microstructure and etc. The reduction effect of deposited carbon was better than that of activated carbon mechanically added. The formation of SiC was precominant over that of Si2ON2 and $\beta$-Sialon owing to low partial pressure of N2 inside the pore, wehreas on the surface of porous glass the formation of Si2ON2 and $\beta$-Sialon were predominant. Thereafter, SiC reduced unreacted glass to be $\beta$-Sialon. Single phase of $\beta$-Sialon(Z=1.92) was obtained from PGA porous glass having the largest pore radius by the simultaneous reduction and nitridation method at 145$0^{\circ}C$ for 5hrs. The bulk density, M.O.R., and KIC of the sitered body are 3.17g/cc, 434.4MPa and 4.1MPa.m1/2, respectively.

• Journal of the Korean Ceramic Society
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• v.29 no.6
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• pp.471-479
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• 1992

AlN powder was synthesized by carbothermal reduction and nitridation using Al2(SO4)3.18H2O as the starting material. The synthesized AlN powder was fine but contained oxygen. Therefore carbonaceous material (carbon black or phenol novolac) was added teogether with the sintering aids (CaO, CaF2, CaCl2, Y2O3 and YF3). It was found that pressureless sintering at 1700~180$0^{\circ}C$ after deoxidation at 150$0^{\circ}C$ suppressed the formation of second phase (27R) and reduced the contents of lattice oxygen within AlN ceramics.