• Title/Summary/Keyword: Carbothermal Reduction Nitridation

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Grain Boundary Behavior and Heat Treatment Effect of AlN Ceramics Prepared from Al-isopropoxide (Al-isopropoxide로부터 AlN 소결체의 입계상 거동 및 열처리 효과)

  • 황해진;이홍림
    • Journal of the Korean Ceramic Society
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    • v.28 no.4
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    • pp.269-278
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    • 1991
  • Fine AlN powder was synthesized by carbothermal reduction and nitridation of alumimun hydroxide prepared from Al-isopropoxide. AlN ceramics with Y2O3 and CaO were prepared by hot-pressing under the pressure of 30 MPa at 180$0^{\circ}C$ for 1 h in N2 atmosphere. Grain boundary behavior and purification mechanism of AlN lattice were examined by heat treatment of AlN ceramics at 185$0^{\circ}C$ for 1-6 h in N2 atmosphere. AlN ceramics without sintering additives showed poor sinterability. However, Y2O3-doped and CaO-doped AlN ceramics were fully densified nearly to theoretical density. As the heat treatment time increased, c-axis lattice parameter increased. This is attributed to the removal of Al2O3 in AlN lattice. This purification effect of AlN attice depended upon the quantity of secondary oxide phase in the inintial stage of heat treatment and the heat treatment time.

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Morphologically Controlled Growth of Aluminum Nitride Nanostructures by the Carbothermal Reduction and Nitridation Method

  • Jung, Woo-Sik
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1563-1566
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    • 2009
  • One-dimensional aluminum nitride (AlN) nanostructures were synthesized by calcining an Al(OH)(succinate) complex, which contained a very small amount of iron as a catalyst, under a mixed gas flow of nitrogen and CO (1 vol%). The complex decomposed into a homogeneous mixture of alumina and carbon at the molecular level, resulting in the lowering of the formation temperature of the AlN nanostructures. The morphology of the nanostructures such as nanocone, nanoneedle, nanowire, and nanobamboo was controlled by varying the reaction conditions, including the reaction atmosphere, reaction temperature, duration time, and ramping rate. Iron droplets were observed on the tips of the AlN nanostructures, strongly supporting that the nanostructures grow through the vapor-liquid-solid mechanism. The variation in the morphology of the nanostructures was well explained in terms of the relationship between the diffusion rate of AlN vapor into the iron droplets and the growth rate of the nanostructures.

Synthesis of $\alpha$-Sialon Ceramics from an Alkoxide and Their Mechanical Properties(II) (알콕사이드로 부터 $\alpha$-Sialon 세라믹스의 제조 및 기계적 성질(II))

  • 이홍림;윤창현
    • Journal of the Korean Ceramic Society
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    • v.28 no.3
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    • pp.189-196
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    • 1991
  • Si(OC2H5)4, commercial AlN and Y2O3 powder were used as the precusor of Si3N4, AlN, Y2O3, respectively. After Si3N4 powder was synthesized by carbothermal reduction and nitridation at 135$0^{\circ}C$ for 13h in N2 atmosphere, characteristics of synthesized powder and the ceramics sintered at 178$0^{\circ}C$ for 1h under 30MPa were investigated. In order to evaluate the reliability of sintered body, Weibull modulus was investigated. Premixing of carbon black as a reduction agent had no effect on Si(OH)4 formation, and Si3N4 powder synthesized from Si(OC2H5)4 was $\alpha$-Si3N4 single phase. Mechanical properties of sintered body were measured as follows : flexural strength ; 750MPa, fracture toughness ; 3.71Mn/3/2, hardness : 17.4GPa, thermal shock resistence temperature ; $600^{\circ}C$. Flexural strength at room temperature was 750MPa and was retained up to 110$0^{\circ}C$. The Weibull modulus of sintered body was 10.7.

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Preparation of Aluminum Nitride from an Alkoxide and its Properties (알콕사이드로부터 AlN분말의 합성 및 분말 특성)

  • 이홍림;박세민;조덕호
    • 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.

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Synthesis of $\alpha$-Sialon Ceramics from an Alkoxide and Their Mechanical Properties(I) (알콕사이드로부터 $\alpha$-Sialon 세라믹스의 제조 및 기계적 성질(I))

  • 이홍림;윤창현;조덕호
    • Journal of the Korean Ceramic Society
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    • v.28 no.2
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    • pp.130-140
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    • 1991
  • The powders of the system Si3N4-Y2O3-AlN were prepared using Si(OC2H5)4 and YCl3.6H2O together with commercial AlN powder. $\alpha$-Si3N4 was prepared by the carbothermal reduction and nitridation of the hydrolyzed gel at 135$0^{\circ}C$ for 10h in N2 atmosphere. YCl3.6H2O was observed to be changed to Y2O3 during the reaction. $\alpha$-Sialon(X=0.2, 0.4, 0.6) ceramics were obtained by hot-pressing the Si3N4-Y2O3-AlN mixture at 178$0^{\circ}C$ for 1h under 30 MPa. The content of $\alpha$-Sialon increased with increasing metal solubility(x value) and $\alpha$-Sialon single phase was obtained at the metal solubility of 0.6. With increasing metal solubility, flexural strength, fracture toughness and thermal shock resistence were decreased, while the microhardness was increased. Large elongated $\beta$-Si3N4 grains were mainly observed at lower metal solubility. Mechanical prorerties of the sintered ceramics with X=0.2 were measured as follows : flexural strength ; 650 MPa, fracture toughness ; 3.63 MN/m3/2, hardness ; 14.7 GPa, thermal shock resistence temperature ; 58$0^{\circ}C$.

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