• Korean Journal of Materials Research
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• v.5 no.7
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• pp.888-896
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• 1995

In this paper the manufacture of shrinkage-free in situ Mullite-ZrO$_2$ceramics through the addition of Al base metal powder to the mixture of ZrSiO$_4$and A1$_2$O$_3$was attempt. The ZrO$_2$-strengthened mullite ceramics was prepared after the following reaction form, 3(Al+Al$_2$O$_3$)+2ZrSiO$_4$longrightarrow3A1$_2$O$_3$.2SiO$_2$+2ZrO$_2$Al metal powder was added from none to 30 weight percent to the A1$_2$O$_3$. The powders were mechanically mixed, isostatically pressed and reaction sintered at 1450-1$600^{\circ}C$ for 3hours. The specimens were sintered with and without intrim soaking time for 5 hours at 125$0^{\circ}C$ for the oxidation of Al-powder The addition of aluminium accelerates the reaction and compensate the shrinkage during the sintering through an increase in volume of oxidized Al. Because coarse flake type Al metal powders were not effectively milled, oxidized Al resulted in the relative large pore in the specimen.

• Journal of the Korean Ceramic Society
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• v.27 no.2
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• pp.201-210
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• 1990

The mullite-15v/o ZrO2 composites were prepared by dispersing ZrO2-3m/o Y2O3 powders into the mullite matrix in order to improve the mechanical properties of the mullite. The densification and retention of t-ZrO2 in the matrix of synthetic mullite were also investigated. From IR spectroscopic analysis, the obtained amorphous SiO2-Al2O3 powder was observed to have Si-O-Al chemical bond in its structure which might result in the homogeneous mullite composition. The lattice parameter of the mullite powder calcined above 130$0^{\circ}C$ (a0=7.5468$\AA$) is nearly close to the value of stoichiometric mullite (71.8wt% Al2O3, a0=7.5456$\AA$). The sintering behavior, microstructure, flexural strength and fracture toughness of the mullite and mullite-15v/o ZrO2 composites have been studied. The mullite-15v/o ZrO2(+3m/o Y2O3) ceramics with relative densities of 96% were obtained when sintered at 1$600^{\circ}C$. The flexural strength and fractrue toughness of the composites sintered at 1$600^{\circ}C$(calcination temperature of mullite powders ; 125$0^{\circ}C$) had maximum values of 307MPa and 2.50MPa.m1/2, respectively. The fracture toughness improvement in the mullite-ZrO2 cmoposite is assumed to be resulted from the combined effect of the stress-induced phase transformation of tetragonal ZrO2 and the crack deflection due to microcracking by the monoclinic ZrO2 formation.

• Journal of the Korean Ceramic Society
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• v.32 no.8
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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${\mu}{\textrm}{m}$.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09a
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• pp.327-328
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• 2006

We have demonstrated that textured $Al_2O_3-mullite-SiC$ nanocomposites can be fabricated by slip casting followed by partial oxidation - reaction sintering of mixed suspensions of $Al_2O_3$ and SiC powders in a high magnetic field. The sintered density was changed by the degree of oxidation at 1200C and 1300C. The degree of orientation of alumina in the nanocomposite was examined on the basis of the X-ray diffraction patterns and scanning electron micrographs. It is confirmed that alumina-oriented nanocomposites were fabricated. The three-point bending strength at room temperature was observed for the nanocomposites.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09a
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• pp.455-456
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• 2006

We have demonstrated that textured $Al_2O_3-mullite-SiC$ nanocomposites can be fabricated by slip casting followed by partial oxidation. reaction sintering of mixed suspensions of $Al_2O_3$ and SiC powders in a high magnetic field. The sintered density was changed by the degree of oxidation at 1200C and 1300C. The degree of orientation of alumina in the nanocomposite was examined on the basis of the X-ray diffraction patterns and scanning electron micrographs. It is confirmed that aluminaoriented nanocomposites were fabricated. The three-point bending strength at room temperature was observed for the nanocomposites.

• Journal of the Korean Ceramic Society
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• v.41 no.4
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• pp.297-301
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• 2004

Nano-sized mullite (3Al$_2$O$_3$$.$2SiO$_2$) colloids were prepared by use of the spray combustion method. For combustion reaction, Al(NO$_3$)$_3$$.$9$H_2O$, and CH$_{6}$N$_4$O were used as an oxidizer and a fuel respectively, and then colloidal silica was also added as 2SiO$_2$source for mullite. The temperature of the reaction chamber was kept at 80$0^{\circ}C$ to initiate the ignition of droplets of the mixed precursors. For preventing droplet coagulation, the droplet number concentration was reduced using the metal screen filter, and the residence time of aerosol was kept at 2.5 seconds for laminar flow. The synthesized colloidal particles had an uniform spherical shape with 130 nanometer size and the crystalline phase showed the mullite with stoichiometry in the observations of XRD and TEM.

• Composites Research
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• v.13 no.5
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• pp.31-36
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• 2000

The effect of several important processing variables was investigated on formation of porous mullite with acicular microstructure. Experimental results demonstrated that microstructure and porosity of porous mullite are depending on concentration of $AlF_3$, holding time at $900^{\circ}C$ and starting material. Acicular mullite was developed by increasing amount of $AlF_3$ and holding time at $900^{\circ}C$. Mullite began to be formed at $1200^{\circ}C$ and the resultant microstructure sintered at this temperature is similar to those at higher temperatures. Porosity increases with increase in amounts of $AlF_3$ and holding time at $900^{\circ}C$ . Therefore, it is found that microstructure of reaction-sintered porous mullite can be controlled by governing the amount of $AlF_3$ and holding time at $900^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.26 no.3
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• pp.347-360
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• 1989

Spinel, mullite, forsterite and cordierite composition powders were synthesized from Mg(NO3)2.6H2O, Al(NO3)3.9H2O and SiCl4-ethanol solution by spray pyrolysis method and the sinterability of these powders were investigated. The bulk density of spinel and mullite specimens sintered at 1,$700^{\circ}C$ for 1hr was 3.56g/㎤(99.5% relative density) and 3.16g/㎤(99.7% relative density), respectively. (Green compacts were made from powders prepared at 1,00$0^{\circ}C$). The bulk density of forsterite and cordierite specimens sintered at 1,480 and 1,40$0^{\circ}C$ for 2hrs were 3.217 and 2.155g/㎤, respectively. (Green compacts were made from powders prepared at 1,00$0^{\circ}C$). The constituent compositions of spinel and mullite specimens sintered at 1,$700^{\circ}C$ for 1hr were 27.5wt% MgO and 70.5wt% Al2O3, respectively. Vickers microhardness and fracture toughness of spinel sintered at the above condition were 13.7GPa and 2.6MN.m3/2, respectively, and room temperature bending strength, 425MPa, was nearly maintained even at the elevated temperature. In the case ofmullite specimens, those values were 13.5GPa, 2.2MN/m3/2 and 430MPa, respectively.

• Journal of the Korean Ceramic Society
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• v.26 no.5
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• pp.625-630
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• 1989

Aluminium silicate gels were prepared by gel-technique using Al(OH)3 and TEOS as starting materials. Aluminium silicate gel as formed mullite at 120$0^{\circ}C$. From this method, homogeneous mullite was formed available needle-like shaped and close compacted. As excess SiO2 mullite composition, the needle-like shaped crystal, size according to increased with SiO2, was increased from 3${\mu}{\textrm}{m}$ to 7${\mu}{\textrm}{m}$ but liquid phase did not affect the formation of needle-like shaped mullite. As excess Al2O3 mullite composition, the needle-shape mullite crystal could not be detected because Al2O3 acted as chunky behavior.

• Journal of the Korean Ceramic Society
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• v.52 no.5
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• pp.374-379
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• 2015

Mullite-matrix and $Al_2O_3$-matrix composites were fabricated with 30 wt% hydroxyapatite (HA) and tricalcium phosphate (TCP), respectively, as additives to give bioactivity. A diphasic gel process was employed to lower the densification temperature of the mullite matrix to $1320^{\circ}C$. A polymer complexation process was used to synthesize a TCP powder that was fully densified at $1250^{\circ}C$, for application to the matrix. For the HA/mullite composite, HA decomposed during sintering by reactions with the matrix components of $Al_2O_3$ and $SiO_2$, resulting in a mixture of $Al_2O_3$, TCP, and other minor phases with a low densification of less than 88% of the theoretical density (TD). In contrast, the TCP/$Al_2O_3$ composite was highly densified by sintering at $1350^{\circ}C$ to 96%TD with no reaction between the components. Different from the TCP monolith, the TCP/$Al_2O_3$ composite also showed a fine microstructure and intergranular fracture, both of which characteristics are advantageous for strength and fracture toughness.