• 한국세라믹학회지
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• 제30권7호
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• pp.571-577
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• 1993

The effect of $\alpha$-Al2O3 seeding on preparation of zirconia/alumina gel fragment prepared by sol-gel processing was characterized through XRD, SEM, TG/DTA and IR analysis. Aluminum isopropoxide and zirconium butoxide were used as starting materials. $\alpha$-Al2O3 seeding restrained grain growth of alumina and zirconia, and decreased tetragonal to monoclinic phase transformation of zirconia on cooling. Therefore, fine zirconia-toughened alumina composite having the relative sintered density of about 98% of theoretical at 140$0^{\circ}C$ for 2h could be obtained.

• 한국세라믹학회지
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• 제25권2호
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• pp.136-142
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• 1988

β-Al2O3, which is used for solid electrolyte membrances in sodium-sulfur batteries, was prepared by sol-gel process. Sodium-n-propoxide NaOC3H7 and aluminum-isopropoxide Al(OC3H7)3 were hydrolyzated in the solution at pH 3, pH 7, pH 9 and pH 11, respectively. The sol-gel processed samples were calcined at several temperature steps, respectively and analysed by thermal analyser(DT-TGA), infrared spectrum analyser and X-ray diffraction analyser. The gelling rate of solution at pH 7 was much higher than that of the solution at pH 3. Thermal exchanging behavior of the gels at pH 3 were similar to Na2O·Al2O3·6H2O and, above pH 7, were similar to Na2O·Al2O3·3H2O. When samples' composition ratio was 9.13 : 90.87 [NaOC3H7:Al(OC3H7)3] at pH 7, β-Al2O3 was formed at 1100℃.

• The Korean Journal of Ceramics
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• 제5권4호
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• pp.379-385
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• 1999

Minute boehmite crystals with high aspect rations, which were hydrothermally synthesized from gibbsite in $Ba(OH)_2$ solution, occluded Ba with the Ba/Al molar ratio of about 0.03 in their interlayers. Their surface areas were about 14$\m^2$/g. The Ba-intercalated bohemite samples were partly used for producing $BaAl_{12}O){19}$ with low sinterability by externally supplementing $Ba(OH)_2$, and for forming transient aluminas. The surface area of $BaAl_{12}O){19}$ obtained by firing at $1500^{\circ}C$ for 3 h was 5.3$\m^2$/g, which was significantly lower than 12$\m^2$/g of the sol-gel origin. While a mixture ${\gamma}$-alumina and BaO is known to from $BaAl_{12}O){19}$ at $1200^{\circ}C$, solid state reaction between η-alumina transformed from the Ba-intercalated boehmite and BaO formed from $Ba(OH)_2$ deposited on the boehmite started above $1300^{\circ}C$. This suggests that large sized $Ba^{2+}$ ion occluded in η-alumina considerably suppresses the diffusion of $Al^{3+}$ ion. The surface area of the Ba-intercalated boehmite fired at $1400^{\circ}C$ for 3h was as high as 14$\m^2$/g indicative of its potential applicability to combustion catalysts. But it was decreased to 5.0$\m^2$/g after firing at $1500^{\circ}C$ for 3 h, accompanied by abrupt formations of $\alpha$-alumina and $BaAl_{12}O){19}$ as main products. The suppression of $\alpha$-alumina formation up to $1400^{\circ}C$ also suggests the significant blocking effect of $Ba^{2+}$ ion on the diffusion of the component ions.

• 한국세라믹학회지
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• 제32권8호
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• pp.909-914
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• 1995

From alumina powder and TEOS, $\alpha$-Al2O3/SiO2 composite powder for reaction-sintered mullite was synthesized by heterogeneous coagulation and surface coating, and investigated the mullitization reaction and sintering behavor of these powders. In $\alpha$-Al2O3/SiO2 composite powder prepared by heterogeneous coagulation, each alumina particles were surrounded by silica particles of 50~60 nm in size. And the alumina particles in composite powder prepared by surface coating were coated by uniform silica layer with thickness of 50 nm. In both methods, mullitization reaction was completed at 1$650^{\circ}C$ for 3h, and specimen sintered above 145$0^{\circ}C$ was about 95% fo the theoretical relative density. Mullite grains formed from the reaction with composite powders showed spherical shape with a size of 1~2${\mu}{\textrm}{m}$.

• 한국결정성장학회지
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• 제12권2호
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• pp.80-86
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• 2002

$Al_{2}O_{3}/SiC$ nanocomposites were made by infiltrating partially sintered alumina bodies with polycarbosilane (PCS) solutions, which is a SiC polymer precursor, with pressureless sintering. The SiC content, densification, phases, strength, and microstructure were investigated with the processing parameters such as PCS solution concentration and heat treatment condition for PCS pyrolysis and sintering. The results were compared with those for pure alumina and nanocomposite samples made by the existing polymer precursor route (i.e. the PCS addition process). The SiC contents of up to 1.5 vol% were obtained by the PCS infiltration. PCS pyrolysis, followed by air heat treatment, was needed before sintering to avoid a cracking problem and to attain a densification as high as 98 % of theoretical. The nanocomposites exhibited significantly higher strength than pure alumina and those prepared by the PCS addition process despite larger grain size. Besides $\alpha-Al_{2}O_{3}/SiC$ and $\beta-SiC$ phases, mullite was present a little in the nanocomposites, which resulted from the reaction of $SiO_{2}$ in the pyrolysis product of PCS with the $Al_{2}O_{3}$ matrix during sintering. The nanocomposites had intagranular particles believed to be SiC, which is a typical feature of $Al_{2}O_{3}/SiC$ nanocomposites.

• 한국세라믹학회지
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• 제31권12호
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• pp.1437-1442
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• 1994

Self propagating synthesis and thermal explosion of combustion reactions were applied to Al/K2Cr2O7/Al2O3 system as the first stage for a production of magnesia-chromium refractory. Several factors related to products made by two combustion reactions were considered and properties of products were characterised. Two processes were required to preheat upto at least 80$0^{\circ}C$ for the thermal explosion and the self propagating synthesis. These processes were so violent and explosive that alumina as diluent was added to the system in order to absorb the reaction heat and reduce the reaction rate. The products consisted of crystal phases of KAl5O8, Cr2O3, Al2O3, K2CrO4, and K2Al2O4.3H2O. The amount of KAl5O8 and K2Al2O4.3H2O crystal phases of products were decreased with further addition of alumina.

• 공업화학
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• 제5권4호
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• pp.597-608
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• 1994

$(NH_4)_2SO_4$와 저품위 bauxite의 황산화 반응에 따라 얻어진 ammonium aluminium sulfate로부터 수열균일침전을 통해 무정형 alumina gel수화물 및 결정형 boehmite를 합성하고 이로 부터 고순도 $Al_2O_3$를 제조하는 새로운 공정 개발을 시도하였다. 이 공정은 ammonium aluminium sulfate용액 중의 Fe 성분을 제거하기 위한 용매추출공정과 정제된 ammonium aluminium sulfate용액으로부터 균일침전에 의한 Al 함유 침전물의 생성에 관한 것으로 이루어져 있다. 추출제 Alamine 336에 의한 적절한 용매추출조건은 shaking time 4분, 수상에 대한 유기상의 비 0.25였다. Urea를 이용한 수열균일 침전반응은 Al 함유용액 중의 Al에 대한 urea의 당량비 6.0의 조건에서 반응온도 $100^{\circ}C$ 이하에서는 무정형 alumina gel 수화물, $120^{\circ}C$ 이상 $150^{\circ}C$ 이하에서는 pseudo boehmite 그리고 $150^{\circ}C$ 이상에서는 결정형 boehmite가 합성되었다. 이 합성된 무정형 alumina gel 수화물은 소성시간 2시간, 소성온도 $1000^{\circ}C$ 이상에서 그리고 결정형 boehnite는 소성시간 2시간, 소성온도 $1250^{\circ}C$ 이상에서 ${\alpha}-Al_2O_3$로 전이되며 얻어진 ${\alpha}-Al_2O_3$의 순도는 99.97%의 고순도였다.

• 한국세라믹학회지
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• 제39권3호
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• pp.272-277
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• 2002

전구체로 ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ 착물을 이용한 수정된 열탄소환원질화법으로 질화알루미늄(AlN) 분말과 휘스커를 합성하였다. 이 분말은 질소분위기에서 별도의 환원용 탄소를 혼합하지 않고 1200$^{\circ}$C에서 1500$^{\circ}$C까지의 온도에서 하소시킨 다름 잔류탄소를 태워 버림으로써 얻어졌다. 이 질화과정을 Al-27 마법각 스핀 핵자기공명, 적외선 분광법 및 X-선 회절법으로 연구했다. 전구체 착물은 열분해되어 ${\rho}$-알루미나와 ${\gamma}$-알루미나로 되었다가 ${\gamma}-{\alpha}$알루미나 전이없이 AlN으로 바뀌었다. ${\gamma}$-알루미나가 AlN으로 바뀌면서 분말의 형상이 유지되는 것으로 보아 이 변환과정에서의 중간체는 알루미늄이나 aluminum suboxides와 같은 기체상이 아니고, 고체상의 $AlO_xN_y$임을 알 수 있다. (0001) 사파이어를 이용하면 AlN 휘스커를 합성할 수 있다.

• 한국세라믹학회지
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• 제32권4호
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• pp.455-461
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• 1995

To investigate the synthesis of $\beta$-Al2O3 and its crystallization behavior by oxalate coprecipitation method, the optimum pH range for oxalate coprecipitates has been theoretically calculated from the solubility products and the equilibrium constans of each metal ionic species and their solubility diagram wa obtained. The optimum pH range for oxalate coprecipitates at room temperature was estimated as <4. In experiment, we found that the optimum condition for oxalate coprecipitates was pH<1, which was not doped with pH controller. The Na+ ions were easily exchanged for the NH4+ ions of NH4OH which was used as pH controller, and those NH4+ ions were supposed to affect the crystallization behavior of $\beta$-Al2O3. The thermal decomposition of all complexes was almost complete below 40$0^{\circ}C$. The primary product of the decomposition process was m-Al2O3, which transformed to $\beta$"- or $\beta$-Al2O3 at temperature higher than 100$0^{\circ}C$. We found that the powder prepared at 120$0^{\circ}C$ had only $\beta$"- and $\beta$-Al2O3.EX>-Al2O3.

• 한국세라믹학회지
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• 제19권2호
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• pp.157-161
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• 1982

The possibility of extraction of alumina from domestic Ha-dong kaolin was studied by sulfuric acid treatment. Raw kaolin was calcined at various temperature (500-110$0^{\circ}C$) and calcined kaolin were treated with sulfuric acid. The tendency of extraction yield of alpha alumina have been investigated by relating reaction time, temperature, and acid concentration. After reaction, precipitates were analyzed by DTA, TGA, and identified alpha alumina by X-ray diffractometer with calcined sample at 120$0^{\circ}C$. The results were as follows; 1. The optimum calcination temperature was 800-86$0^{\circ}C$. 2. The most suitable extracting conditions of alpha alumina were 40 wt%-$H_2SO_4$, 2-3 hours acid-treating time and 8$0^{\circ}C$ acid-treating temperature. 3. Precipitates were composed of $(NH_4)_2SO_4$, $Al_2SO_4(OH)_4$ 5-7 $H_2O$ and $Al(OH)_3$.