• 한국세라믹학회지
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• 제25권6호
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• pp.585-592
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• 1988

Aluminum sec-butoxide was synthesized from aluminum foil and alcohol. The characteristics of the alumina powder prepared from the synthesized alkoxide by the Yoldas method were studied. As a result of measuring the synthesized aluminum sec-butoxide by GC, the purity of the synthesized alkoxide was 98.7% on the basis of commercial alkoxide and the yield was 78.5%. A127-MASNMR analysis shows that powders dried at 9$0^{\circ}C$ and $\alpha$-Al2O3 have 6-cordinated structure and ${\gamma}$-Al2O3 has 4-coordinated structure. The characteristics of alumina powder prepared from the synthisized alkoxide showed the same characteristics with the alumina powder prepared from the commercial alkoxide.

• 한국세라믹학회지
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• 제26권5호
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• pp.593-600
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• 1989

Fine spinel powder was prepared from the Mg-Al double alkoxide synthesized using magnesium powder, aluminum foil and sec-butyl alcohol. This powder was compared with powder prepared by mixing two commercial alkoxides. The spinelization was started at 50$0^{\circ}C$ and was almost completed at 100$0^{\circ}C$ with a good crystallinity in the double alkoxide system. In mixed alkoxide system, homogeneous spinel powder was not obtained and MgO existed as a second phase because of solubility and hydrolysis rate differences of two alkoxides. The relative density of specimen prepared by double alkoxide was 99% and specimen prepared by mixed alkoxide was 95%. The modulus of rupture of specimens prepared by double alkoxide and mixed alkoxide was 49.9kg/$\textrm{mm}^2$ and 41.6kg/$\textrm{mm}^2$, respectively.

• 한국세라믹학회지
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• 제33권3호
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• pp.348-354
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• 1996

• The Korean Journal of Ceramics
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• 제1권3호
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• pp.137-142
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• 1995

Monodispersed $Al_2O_3-TiO_2$ Powder was prepared by metal-alkoxide hydrolsis. A homogeneous nucleation/growth occurred in the solutions containing ethanol, butanol and acetonitrile, and resulted in spherical, submicrometer-sized powder. The titania and the alumina crystals were formed at $800^{\circ}C$ and $1000^{\circ}C$, respectively. These crystala were subsequently reacted each other beyond $1320^{\circ}C$ and formed $Al_2TiO_5$. The relative densities of sintered bodies prepared with as-received powder were examined at the temperature range of 1300-$1500^{\circ}C$ and they were about 79% at $1300^{\circ}C$. The formation of aluminum titanata decreased the relative density at the temperature range of 1300-$1450^{\circ}C$, and at above $1450^{\circ}C$, the relative density started to increase again. It was observed that $\alpha-Al_2O_3$-doped aluminum titanate was more stable than pure aluminum titante at $1200^{\circ}C$.

• 한국세라믹학회지
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• 제25권3호
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• pp.217-224
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• 1988

Alkoxide 법으로 합성한 알루미나의 동공 구조를 BET 법으로 구한 흡 탈착 등온선의 hysteresis loop와 동공 분포로부터 고찰하였다. 알루미나는 aluminum isopropoxide를 화학량의 물로 가수분해하여 제조하였고, 가수분해 온도는 3$^{\circ}C$와 8$0^{\circ}C$에서 수행하였다. 이어 20$0^{\circ}C$부터 50$0^{\circ}C$까지 단계적으로 승온시키며 일정시간 열처리하였다. 3$^{\circ}C$ 가수분해 시료의 동공부피는 열처리 온도에 비례하여 증가하였으며, 동공크기는 쌍입분포(twin peaked pore size distribution)형으로 나타났다. 그러나 8$0^{\circ}C$ 가수분해 시료는 열처리에 의하여 동공부피가 감소하고, 동공크기는 단입분포(single peaked pore size distribution)로 나타났다. 이러한 관찰 결과로부터 전자의 동공형태는 slit형, 후자는 ink-bottle형을 하고 있는 것으로 추정되었다. 이와 같이 가수분해 온도는 동공 형태를 결정하는 중요한 인자일 뿐만 아니라, 층상 알루미나의 구조수 일탈 거동을 결정하는데 중요하다. 열처리 효과는 단지 최종 제품의 동공 분포를 결정하는데 영향을 주고 있는 것으로 해석되었다.

• 대한화학회지
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• 제33권2호
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• pp.263-270
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• 1989

금속알루미늄 조각과 alcohols을 반응시켜 Al-alkoxides를 합성하였으며 이것을 가수분해하여 얻은 Al-hydroxides와 시약 AlCl3로부터 얻은 Al-hydroxides를 여러 온도에서 소성하여 여러 상의 고순도 $Al_2O_3$를 제조하였다. 제조한 ${\gamma}$와 ${\eta}$상 알루미나의 촉매적 특성을 알아보았고, $Al(OH)_3$로부터 ${\alpha}-Al_2O_3$의 생성과정을 속도론적으로 고찰하였다.

• 한국세라믹학회지
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• 제35권9호
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• pp.953-957
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• 1998

The effects of catalysts and reactive conditions on the synthesis of aluminum alkoxides are investigated. HgCl2 and I2 as catalysts are used in the synthesis reaction for comparing to no addtion. The absorption peak in IR spectra according to Al-O-L bond of aluminum isopropoxide and aluminum sec-butoxide appear at near 1030cm-1 and 1060cm-1 respectively regardless of kinds of catalysts. The synthesis yield of alu-minum-isopropoxide was 90% in case of no catalyst addition and increased to all of 95% by addition of HgCl2 and I2 The synthesis yield of aluminum sec-butoxide is increased to 95% by addition of I2 catalyst com-paring to no addition.

• 한국세라믹학회지
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• 제31권11호
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• pp.1271-1282
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• 1994

The surface of commercial alumina fibers used for reinforcing the MCFC matrix has been coated with ${\gamma}$-LiAlO2 being the same material as the matrix, by the sol-gel method in order to enhance the corrosion resistivity of alumina fibers. Stable LiAlO2 complex polymeric sols for coating was synthesized by mixing aluminum alkoxide polymeric sols with LiNO3 solution. It was found that the LiAlO2 polymeric sol prepared by adding the mixed chelate of acethylacetone and triethanolamine (the mole ratio of AA/TEA = 0.125/0.75) to the 1 mole of the aluminum alkoxide had the excellent stability and coating behavior. The crystalline structure of the dried gel from the ${\gamma}$-LiAlO2 sol was completely transformed into the ${\gamma}$-LiAlO2 at $600^{\circ}C$. The optimum viscosity of the sol for coating the alumina long fibers was 30~40 cP, while it was 12~20 cP in case of the short fiber coating. The ${\gamma}$-LiAlO2 coated alumina fibers without defects fully densified when heat-treated at 120$0^{\circ}C$.

• 한국세라믹학회지
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• 제26권1호
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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.

• 한국재료학회지
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• 제3권4호
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• pp.372-380
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• 1993

탄소/탄소 복합재의 산화 저항성을 개선시키기 위하여 aluminum iso propoxide및 aluminum tri sec butoxide졸을 2D-탄소/탄소 복합재에 도포하여 산호 억제층으로서의 효과를 관찰하였다. 촉매/알콕사이드의 몰비가 0.07, 물/알콕사이드의 몰비가 100일때의 산화 억제효과가 양호했으며, 승온속도를 $20^{\circ}C$/min로 하여 승온분석시험한 결과는 도포시편이 $80^{\circ}C$ 정도의 산화 개시온도가 20%감소되는 시간을 측정한 TGA분석에서는 도포시편이 20% 정도의 산화 저항성 개선효과를 나타냈다. 도포막의 두께는 1회 도포막이 3${\mu}$m, 2회 및 3회 도포막이 4-5${\mu}$m 정도였고, 열충격 시험은 횟수에 따라 산화량이 증자하였다. 5% 전환률에서의 도포하지 않은 시편의 활성화 에너지는 33.2Kcal/mole이었으며 도포시편의 활성화 에너지는 37.1Kcal/mole이었다.