• Journal of the Korean Ceramic Society
• /
• v.30 no.7
• /
• pp.571-577
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.25 no.2
• /
• pp.136-142
• /
• 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
• /
• v.5 no.4
• /
• pp.379-385
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.32 no.8
• /
• pp.909-914
• /
• 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${\mu}{\textrm}{m}$.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.12 no.2
• /
• pp.80-86
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.31 no.12
• /
• pp.1437-1442
• /
• 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.

• Applied Chemistry for Engineering
• /
• v.5 no.4
• /
• pp.597-608
• /
• 1994

A new process for the production of high purity ${\alpha}-Al_2O_3$ from ammonium aluminium sulfate solution abtained through the sulfation of low grade bauxite ore with $(NH_4)_2SO_4$, and leaching of the sulfated product was investigated. This process is consisted of solvent extraction for Fe component removal from ammonium aluminum sulfate solution and homogeneous precipitation of Al containing precipitate from the refined ammonium aluminium sulfate solution by using urea as precipitator. The optimum conditions of solvent extraction with Alamine 336 as extractant were shaking time of 4min, organic phase ratio to aqueous phase of 0.25. The types of precipitation products from this precipitation were amorphous alumina gel, pseudo-boehmite and crystalline boehmite in the lower temperature of $100^{\circ}C$, in the range from $125^{\circ}C$ to $150^{\circ}C$, and above $150^{\circ}C$, respectively. And also amorphous alumina gel hydrate in $1000^{\circ}C$ and crystalline boehmite in $1250^{\circ}C$ were tranfered to ${\alpha}-Al_2O_3$, respectively. This alumina was identified as ${\alpha}-Al_2O_3$ of purity 99.7%.

• Journal of the Korean Ceramic Society
• /
• v.39 no.3
• /
• pp.272-277
• /
• 2002

Aluminum nitride (AlN) powders and whiskers were synthesized by a modified carbothermal reduction and nitridation where a ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ complex is used as precursor. The AlN powders were obtained by calcining the complex without mixing any carbon source under a flow of nitrogen in the temperature range 1200∼1500$^{\circ}$C and then burning out the residual carbon. The nitridation process was investigated by $^{27}Al$ magic-angle spinning (MAS) unclear magnetic resonance, infrared spectroscopy and X-ray diffraction. The complex is pyrolyzed, converted to ${\rho}$- and ${\gamma}$- alumina and then nitridated to AlN without ${\gamma}-{\alpha}$ alumina transition. The morphology of ${\gamma}$-alumina, when it was converted to AlN, was retained, strongly indicating that ${\gamma}$-alumina is converted to AlN through solid-state $AlO_xN_y$, not through gaseous intermediates such as aluminum and aluminaum suboxides. AlN whiskers were obtained, when a (0001) sapphire was used as a catalyst.

• Journal of the Korean Ceramic Society
• /
• v.32 no.4
• /
• pp.455-461
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.19 no.2
• /
• pp.157-161
• /
• 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 $Al(OH)_3$.