• Journal of the Korean Ceramic Society
• /
• v.28 no.5
• /
• pp.365-372
• /
• 1991

LAS (lithium aluminosilicate) sol was synthesized using the hydrolysis-condensation reaction of TEOS, chelated Al(OBus)3 and Li-salt with H2O in alcohol (EtOH+2-Propanol) medium. Effects of important reaction parameters on the properties of sol and gel-derived LAS were examined. The crystallization of the sol-gel derived LAS with ${\beta}$-spodumene composition began at ∼600$^{\circ}C$, and a series of polymorphic transformations occurred as temperature was increased to 1100$^{\circ}C$: amorphous LAS\longrightarrowhexagonal LiAl(SiO3)2\longrightarrow${\beta}$-spodumene. Lowering Li content in the gel enhanced densification and retarded the crystallization significantly. Optimum reaction conditions of LAS sol formation for thin coating applications were derived from rheological measurements, and these can be summarized as: H2O/total alkoxides molar ratio=4, pH=∼2.5, and aging time of ∼250h.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.21 no.5
• /
• pp.218-224
• /
• 2011

LAS ($Li_2O-Al_2O_3-SiO_2$) ceramics were sintered by a solid-state reaction. $CaCO_3$ and $ZrO_2$ were added to the ${\beta}$-spodumene ($Li_2O-Al_2O_3-4SiO_2$) composition of the LAS system for enhancement of sintering behavior and mechanical strength, respectively. We have investigated the sintering characteristics, microstructures, mechanical properties and thermal expansion characteristics according to the change of the amount of additive and sintering temperature of the ${\beta}$-spodumene. At 0.1 mol% $CaCO_3$, the densification of ${\beta}$-spodumene was significantly improved. At 0.04 mol% $ZrO_2$, the strength of ${\beta}$-spodumene was also improved. For all the selected all compositions, the thermal expansion coefficient was measured by a dilatometer, which revealed 1.2 to $1.7{\times}10^6/^{\circ}C$.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.22 no.1
• /
• pp.57-63
• /
• 2012

$Al_2TiO_5$ ceramics were sintered by a solid-state reaction. LAS (${\beta}$-spodumene) and $Fe_2O_3$ were added to the $Al_2TiO_5$ composition for enhancement of sintering behavior such as mechanical strength and thermal shock resistance. The sintered body was much densified by addition of LAS and $Fe_2O_3$ because LAS formed the liquid-phase and $Fe_2O_3$ suppressed the grain growth. We have systematically investigated the sintering characteristics, microstructures, mechanical properties, and thermal shock resistance according to the change of the amount of additive. When the additive of LAS (20 wt%)-$Fe_2O_3$ was added to $Al_2TiO_5$, it confirmed that superior mechanical properties of the fracture strength of over 120 MPa and the thermal shock resistance of over $1,200^{\circ}C$ were achieved.

• Journal of Powder Materials
• /
• v.18 no.1
• /
• pp.35-40
• /
• 2011

LAS-system ceramic powder, spodumene ($Li_2O{\cdot}Al_2O_3{\cdot}4SiO_2$), was successfully synthesized by a chemical solution technique employing PVA(polyvinyl alcohol) as an organic carrier. The PVA content affected the microstructure of porous precursor gels and the crystalline development. The optimum PVA content contributed to homogeneous distribution of metal ions in the precursor gel and it resulted in the synthesis of glass free $\beta$-spodumene powder having a specific surface area of $7.57\;m^2/g$. The agglomerated $\beta$-spodumene powders were also enough soft to grind to fine powders by a simple ball milling process. The microstructures of the densified powder compacts were strongly dependant on the minor phases of spodumene solid solution and amount of liquid phase, which were formed from the inhomogeneous precursors.

• Journal of the Korean Ceramic Society
• /
• v.29 no.7
• /
• pp.533-538
• /
• 1992

Effect of Li2O.4B2O frit on the microstructural and thermal expansion behaviour of $\beta$-spodumene ceramics was investigated. With 4.0~8.0 wt.% frit addition, sintering temperature range was enlarged and densification was enhanced through liquid phase sintering. As the amount of frit addition was increased, thermal expansion coefficient was increased to 1.72$\times$10-6$^{\circ}C$-1 of its highest value, which indicated that the increment of thermal expansion coefficient due to the second phase was constrained.

• Journal of the Korean Ceramic Society
• /
• v.29 no.8
• /
• pp.646-650
• /
• 1992

Effect of Li2O.4B2O3 frit addition on microstructural and thermal expansion behaviour of the $\beta$-spodumene ceramics made from kaolinite was investigated. With 2.0~4.0 wt% frit addition, the densification by liquid phase sintering caused low water absorption below 3% and enhancement of beding strength. As the amount of frit addition was increased, thermal expansion coefficient was increased to large scale, but in 2 wt% frit addition, its thermal expansion coefficient was constrained to 1.92$\times$10-6$^{\circ}C$-1.

• Journal of the Korean Ceramic Society
• /
• v.31 no.7
• /
• pp.784-794
• /
• 1994

Though spodumene have a law theraml expension and good thermal shock resistance, its sintering temperature is too close to its melting point in the application for industral purpose. Solving the problems, impurities within the silicate minerals act as a frit during firing, so its densification is expected through enlargement of sintering temperature range. By the heat treatment of starting materials, mixtures of silicate mineral, lithium carbonate, if necessary SiO2 or Al2O3 were added for stoichiometric correction, in the range of 1000~125$0^{\circ}C$ for 10 hrs, $\beta$-spodumene single phase was synthesized. Mixtures with sillimanite group minerals, $\beta$-spodumene was formed at 120$0^{\circ}C$ or 125$0^{\circ}C$ via intermediate phases of petalite, Li2SiO3 and LiAlO2. For the case of kaolin group minerals, synthesis were completed at 110$0^{\circ}C$ for Hadon pink kaolin, 120$0^{\circ}C$ for New Zealand white kaolin, When pyrophyllite group minerals were used, those were at the range of 1000~125$0^{\circ}C$. Spodumene was completed at lowest temperature, 100$0^{\circ}C$ from the mixture of Wando pyrophyllite among them. Microstructure of synthesized powders showed the inrregular lump shape such as densed crystallines.

• Journal of the Korean Ceramic Society
• /
• v.28 no.11
• /
• pp.865-872
• /
• 1991

LAS (lithium aluminosilicate) sol was synthesized using the hydrolysis-condensation reaction of TEOS, chelated Al(OBus)3 and LiNO3 with H2O in alcohol (ethanol+2-propanol) medium. Lowering Li content by a factor of 1/2 significantly enhanced densification and retarded the crystallization of LAS gel by ~30$0^{\circ}C$. Dense LAS specimen with essentially pore-free microstructure was obtained by sintering the sol-gel derived gel at 80$0^{\circ}C$ for 4 h and annealing at 120$0^{\circ}C$ for 2 h. Similary, a mixed colloidal processing was attempted as a convenient, alternative route for the fabrication of dense LAS sintered body. The $\beta$-spodumene seeding (~0.8 ${\mu}{\textrm}{m}$) in the sol-gel derived LAS modified the sequence of phase transformations and lowered the temperature of crystallization by ~12$0^{\circ}C$. Combining the epitaxial seeding with the sol-gel process, we could lower the crystallization temperature to the sintering temperature range (~80$0^{\circ}C$) and, demonstrate a possibility of making the viscous sintering/crystallization as a continuous as a continuous unit process.

• Journal of the Korean institute of surface engineering
• /
• v.27 no.2
• /
• pp.99-108
• /
• 1994

Films of glass-ceramics $Li_2O-Al_2O_3-SiO_2$(LAS)system were prepared on substrate of an iron plate(SCP) by sol-gel technique using metal alkoxide such as Si$(OC_2H_5)_4$,Al$(OC_2H_9)_3$) and Ti$(OC_2H_6)_4$). Sol which was made by means of simple spray coating, on the substrate was hydrolyzed at 75~$80^{\circ}C$ in moisture cabinet (80~90 % humidity) to form the multicomponent gel. The films up to about 0.8~1.0$mu extrm{m}$ in thickness can be obtained by repeating operation, spraylongrightarrowhydrolysis and condensationlongrightarrowdryinglongrightarrowheating and crystallization at $700^{\circ}C$ for 3~5min. The far-infrared radiation spectra of the coated films on substrate were examined by FT-IR and of films was also observed by scanning electron micrograph technique. The thermal evaluation of the gel-film is followed by TG/DTA measurements. The structure evaluation is followedd X-ray diffraction. These results suggest that this process is applicable to far-infrared radiat at thin film technique.

• Journal of the Korean Ceramic Society
• /
• v.31 no.5
• /
• pp.572-580
• /
• 1994

With low thermal expansion coefficients, eucryptite (Li2O.Al2O3.2SiO2) and spodumene (Li2O.Al2O3.4SiO2) in LAS ceramic system show good thermal shock resistance. In this study, sillimanite or kaolin group silicate minerals and Li2CO3 were used as starting materials, and if necessary SiO2 or Al2O3 were added for making stoichiometrically formed specimens. By this process, eucryptite powders were synthesized and characterized. The powder mixtures of lithiumcabonate and silicate minerals calcined at 80$0^{\circ}C$ for 2 hrs were made into powder compacts. $\beta$-Eucryptite single phase was formed via intermediate phases of Li2SiO3 and LiAlO2 et al, by heating at 110$0^{\circ}C$ or 120$0^{\circ}C$ for 10 hrs from those powder compacts. When using the sillimanite group minerals, Virginia kyanite or andalusite was reacted to form eucryptite at 120$0^{\circ}C$and CMK International kyanite were completed at 110$0^{\circ}C$. When kaolin group minerals were used, it was found that the synthesizing temperature (100$0^{\circ}C$) of $\beta$-eucryptite from the mixture of New Zealand white kaolin was lower than that from Hadong pink kaolin (110$0^{\circ}C$). The Microstructure of systhesized powder showed the irregular lump shape such as densed crystallines.