• Journal of the Korean Ceramic Society
• /
• v.33 no.8
• /
• pp.915-920
• /
• 1996

Fine mullite precursor was prepared by colloidal sol-gel processes. Aluminum isopropoxide $[Al(i-OC_3H_7)_3]$ as a starting material of $Al_2O_3$ and silicic acid extracted by THF from sodium silicate as a starting material of $SiO_2$ were used. Sodium silicate was first acidified by dilute sulfuric acid to form silicic acid. ; followed by extraction using THF, Mullite precursor was synthesized by sol-gel processes from aluminum isopropoxide and sillicic acid considering the degree of extraction of Si and the removal efficiency of Na. The impurity content of silicic acid extracted by THF was below 0.04% Synthetic mullite precursor consisted of $3Al_2O_3{\cdot}2SiO_2$ and showd spherical particles of $0.05{\mu}m$ diameter and below 0.462% of impurites. The mullite precursor was characterized by EDS, XRD, TG/DSC SEM, FT-IR spectroscopy ICP and TEM.

• The Korean Journal of Ceramics
• /
• v.5 no.2
• /
• pp.137-141
• /
• 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.

• Korean Journal of Materials Research
• /
• v.12 no.7
• /
• pp.573-579
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.37 no.2
• /
• pp.174-180
• /
• 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.

• Korean Journal of Materials Research
• /
• v.13 no.4
• /
• pp.251-258
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.33 no.6
• /
• pp.679-685
• /
• 1996

• Journal of the Korean Ceramic Society
• /
• v.28 no.7
• /
• pp.503-508
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.37 no.6
• /
• pp.517-523
• /
• 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.

• Applied Chemistry for Engineering
• /
• v.4 no.3
• /
• pp.497-504
• /
• 1993

The effect of DCCA (Drying Control Chemical Additives) on the drying of gel was investigated in order to determine an optimum drying condition of mullite precursor through sol-gel process. Aluminium sec-butoxide was synthesized from aluminium foil and then mullite powders were synthesized from Tetra-ethyl-ortho-silicate (TEOS) and the aluminium sec-butoxide. N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane, and Oxalic acid were used as DCCA. Mullite powders that were calcined at 200, 900, 1100, and $1250^{\circ}C$ for 2hr were analysed by XRD, TG-DTA, FT-IR, and SEM in order to investigate structural change and characteristics of calcined powders. The results of this work showed that the drying time of gel was reduced to about half in the presence of 0.1mol DMF compared with the absence of DCCA and also calcined powders were obtained without remarkable structural change despite of the addition of DCCA.

• Proceedings of the Korean Ceranic Society Conference
• /
• 2003.04a
• /
• pp.81.2-81
• /
• 2003