• 한국세라믹학회지
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• 제33권8호
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• pp.915-920
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• 1996

콜로이드 졸-겔법에 의해 초미립자 mullite 분말을 제조하였다. Al2O3의 출발 물질로 aluminum isopropoxide $[Al(i-OC_3H_7)_3]$을, $SiO_2$ 출발 물질로 규산 나트륨으로부터 tetrahydrofuran(이후 THF로 약기함)으로 추출한 규산을 사용하였다. 규산 나트륨은 규산을 생성시키기 위하여 묽은 황산으로 산성화시킨 다음 THF로 추출하였다. Mullite 분말은 졸-겔법에 의해서 Si 추출율와 Na 제거율을 조사한 규산과 aluminum isopropoxide로 부터 합성되었다. THF로 추출한 규산의 불순물 함량은 0.04% 이하이었다. 합성된 mullite 분말은 $3Al_2O_3{\cdot}2SiO_2$ 조성을 갖고 불순물의 함량은 0.0462% 이하의 직경 $0.05{\mu}m$ 정도의 결정상이었다. EDS, XRD, TG/DSC, SEM, FT-IR, ICP, TEM등으로 mullite 분말의 특성을 조사하였다.

• The Korean Journal of Ceramics
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• 제5권2호
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• pp.137-141
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• 1999

To increase the strength of high-purity porous mullite ceramics, ultra fine mullite precursor powders of about 10nm in diameter were deposited at point of contact between primary coarse mullite particles of about 60$\mu\textrm{m}$. The deposited and hetero coagulated structures of ultra fine mullite precursor powders were controlled by pH. The optimum pH condition to form a uniform deposition of mullite powders between coarse mullite particles was in the range from 7 to 8. Deposition of the ultra fine powders did not form at pH < 7 and pH > 10 irregular deposition was observed from pH 8 to 9.

• 한국재료학회지
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• 제12권7호
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• pp.573-579
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• 2002

Stoichiometric mullite ($3Al_2$$O_3$. $2SiO_2$) precursor sol has been prepared by sol-gel method. The effects of the precursor pH and sintering temperature on the synthesizing behavior and morphology of mullite have been studied. Mullite precursor sol was prepared by dissolution of aluminum nitrate enneahydrate (Al($NO_3$)$_3$.9H$_2O) into the mixture of silica sol. Precursor pH of the sols was controlled to acidic condition ($PH\leq$ 1~1.5) and to basic condition ($pH\geq$8.5~9). The synthesized aluminosilicate sols were formed under 20 MPa pressure after drying at $150^{\circ}C$ for 24 hours, and then sintered for 3hours in the temperature range of $1100~1600^{\circ}C$. From TGA/DTA analysis, total weight loss in the aluminosilicate gel of the acidic sample was (equation omitted) 56% and that of the basic sample was (equation omitted) 85%, indicating that the synthesizing temperature of mullite phase for acidic and basic samples was above $1200^{\circ}C$ and $1300^{\circ}C$, respectively. The morphologies of the synthesized mullite were fine and needle-like (or rod-like) for acidic sample, and granular for basic sample that has been sintered above $1300^{\circ}C$. It was found that the morphology of mullite particle was predominantly governed by precursor pH and sintering temperature.

• 한국세라믹학회지
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• 제37권2호
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• pp.174-180
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• 2000

Y-TZP/mullite composites were prepared by the infiltration of Y-TZP precursor into partially reaction-sintered mullite. The addition of Y-TZP(~7.2 wt%) increased the bend strength(207 MPa), fracture toughness(4.6MPa.m1/2) and Vickers microhardness(853kg/$\textrm{mm}^2$) of the uninfiltrated mullite sintered at 162$0^{\circ}C$ for 10h by more than 75, 70 and 105%, respectively. Residual alumina-rich glass was observed at a mullite/mullite junction, due to the mullitization reaction of silica melt with crystalline $\alpha$-Al2O3 during a final sintering. Although ZrO2 inclusions improved the final sintered density of mullite they did not effectively prevent its grain growth.

• 한국재료학회지
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• 제13권4호
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• pp.251-258
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• 2003

The effects of the salt and the precursor pH on the synthesizing behavior and the morphology of mullite have been studied. Two kinds of mullite precursor sols were prepared by the dissolution of two kinds of salt (aluminum nitrate enneahydrate, Al($NO_3$)$_3$ㆍ$9H_2$O; type I and aluminum sulfate 14∼18 water, (SO$Al_4$)$_3$$\cdot$$14∼18H_2$O; type II) into the mixture of colloidal silica sol, respectively. Precursor pH of the sols was controlled to the acidic (pH= 1.5∼2) and basic (pH= 8.5∼9) conditions. The co-products with nitrate and sulfate were completely eliminated at $500^{\circ}C$ and $850^{\circ}C$, respectively, which was confirmed by TG/DTA results. The synthesizing temperature of mullite phase was found to be above $1200^{\circ}C$ for pH= 1.5∼2 and above $1300^{\circ}C$ for pH= 8.5∼9 in type I. However, in type II, the synthesizing temperature of mullite was decreased to $850^{\circ}C$ for pH= 1.5∼2 and $1100^{\circ}C$ for pH= 8.5∼9. The grain size of the mullite synthesized at pH= 8.5∼9 was larger than that at pH= 1.5∼2 in overall heat-treated temperatures, showing smaller grain size in type II. Aspect ratio of the mullite grains was more increased at pH= 1.5∼2 than pH= 8.5∼9 in type I, showing similar aspect ratio at both pH conditions in type II. It was found that the synthesizing temperature and grain size were predominantly governed by the initial precursor pH and decomposition of the salt, with minor effect on the grain morphology.

• 한국세라믹학회지
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• 제33권6호
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• pp.679-685
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• 1996

• 한국세라믹학회지
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• 제28권7호
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• pp.503-508
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• 1991

High pure and fine mullite powders were synthesized from Al-secbutoxide[Al(OC4H9)3] and TEOS[Si(OC2H5)4] (SiO2/Al2O3=2/3 mole). Sol-Gel process by partial hydrolysis technique, as it were, first, TEOS was partially hydrolysized and then mixed with Al-secbutoxide for complete hydrolysis was used. The mullite precursor was synthesized within 30 hrs, which was reduced about a half of synthetic time in comparison with the other's study. Al-Si spinel was formed at 980℃ and mullite crystal was formed at 1200℃. Mullite powders synthesized in this study was spherical type like those of the other studies and particle sizes were very fine. Also mullite powders calcined at 1,600℃ had a stoichiometric composition (3Al2O3·2SiO2) and lattice constants were coincided with known theoretical values.

• 한국세라믹학회지
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• 제37권6호
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• pp.517-523
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• 2000

Effect of catalysts, which was catalyzed by acid(HCl and HNO3) and base(NH4OH), on characteristics of the mullite powders prepared by sol-gel methdo wa sinvestigated by XRD, TGA, SEm AND BET. As a result, weight loss as a function of catalysts was in order of HCl=32.6%>HNO3=25.44%>Non=24.0%>NH4OH=22.5%. The mullite powder dried at 100$^{\circ}C$ appeared spherical shape in acid catalyst and different shape in base catalyst, but sintering powder at 1400$^{\circ}C$ appeared very fine particle of 0.05∼0.1$\mu\textrm{m}$ regardless of catalysts. In all cae, the pore quantity, which was capable to adsoprtion, was decreased with increasing temperature. In base catalyst, no change of special surface area in mullite appeared.

• 공업화학
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• 제4권3호
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• pp.497-504
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• 1993

본 연구는 고온 구조재료 및 전자재료로 주목받고 있는 복합산화물인 mullite($3Al_2O_3${\cdot}2SiO_2$)를 금속알콕사이드에 의한 졸-겔법으로 합성함에 있어서 재활용품으로서의 aluminium foil을 aluminium 금속원으로 사용하여 알루미늄 알콕사이드를 제조하고 $Si(OC_2H_5)_4$와 혼합하여 가수분해 단계에서 건조조절화학첨가제(Drying Control Chemical Additives, DCCA)를 첨가함으로써 건조시간을 단축시키려는 시도를 하였으며 이러한 DCCA가 mullite 물성에 어떠한 영향을 주는지 검토하고자 하였다. 이때 DCCA로 N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane과 Oxalic acid가 첨가되었으며 건조된 겔을 각 온도별로 소성하여 TG-DTA, FT-IR, XRD 및 SEM을 사용하여 결정의 전이과정 및 각 소성온도에서의 결정상태 등을 관찰하였다. DCCA를 첨가하여 건조시킨 결과 0.1mole의 DMF를 첨가하였을 경우 DCCA를 첨가하지 않았을 때보다 건조시간이 1/2 정도 단축되었으며 분석결과 mullite의 결정형성에 큰 영향을 미치지 않았음을 확인하였다.

• 한국세라믹학회:학술대회논문집
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• 한국세라믹학회 2003년도 춘계총회 및 연구발표회 초록집
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• pp.81.2-81
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• 2003