• Journal of the Korean Ceramic Society
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• v.42 no.4
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• pp.282-286
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• 2005

Leucite crystal has been utilized for dental porcelain due to its high thermal expansion coefficient to meet its counter metal side. Many industrial applications of leucite from the incongruently melting of potassium feldspar are used and its minimum temperature of crystallization is $1150^{\circ}C$. This study aimed to get leucite crystal from lower temperature through congruently melting, and the starting materials are taken from K-feldspar mainly, and aluminum hydroxide and potassium carbonate are additionally supplied to meet stoichiometry of leucite. We report that the leucite crystal can be synthesized in congruently melting from the temperature $950^{\circ}C$ through solid-state sintering with k-feldspar, potassium carbonate and aluminum hydroxide.

• Journal of Technologic Dentistry
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• v.31 no.4
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• pp.25-30
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• 2009

Zirconia($ZrO_2$) has attracted much attention in science and technology because of its high refractive index, high melting temperature, hardness, low thermal conductivity and corrosion barrier properties. And it is widely used as the dental restoration material because of its esthetic appearance. In this research, we analyzed the particle size and composition of the imported dental porcelain for zirconia. And the glass frit was produced. To decrease the glass transition temperature and softening temperature of the glass frit, $Li_2O$ was added into it and the effect of $Li_2O$ on the firing temperature was researched. Then the glass which contains leucite crystal with a high coefficient of thermal expansion(CTE) was manufactured and it was mixed with the glass frit to control the CTE. The phase composition were analyzed using the X-ray diffraction. The morphologies of the samples were observed by the scanning electron microscope. The 4wt% $Li_2O$-added glass frit has the optimal glass transition temperature and softening temperature. And 6 wt% leucite crystal was mixed with the glass frit to control the CTE. From the experimental results of crystallization, the crystal phase was found only leucite crystal.

• Journal of dental hygiene science
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• v.18 no.1
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• pp.42-49
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• 2018

The computer-aided design/computer-aided manufacturing (CAD/CAM) system was introduced to shorten the production time of all-ceramic restorations and the number of patient visits. Among these types of ceramic for dental CAD/CAM, they have been processed into inlay, onlay, and crown shapes using leucite-reinforced glass-ceramics to improve strength. The purpose of this study was to observe the mechanical properties and microstructure of leucite-reinforced glass-ceramics for dental CAD/CAM. Two types of leucite-reinforced glass-ceramic blocks (IPS Empress CAD, Rosetta BM) were prepared with diameter of 13 mm and thickness of 1 mm. Biaxial flexural testing was conducted using a piston-on-three-ball method at a crosshead speed of 0.5 mm/min. Weibull statistics were used for the analysis of biaxial flexural strength. Fracture toughness was obtained using an indentation fracture method. Specimens were observed by field emission scanning electron microscopy to examine the microstructure of the leucite crystalline phase after acid etching with 0.5% hydrofluoric acid aqueous solution for 1 minute. The results of strength testing showed that IPS Empress CAD had a mean value of $158.1{\pm}8.6MPa$ and Rosetta BM of $172.3{\pm}8.3MPa$. The fracture toughness results showed that IPS Empress CAD had a mean value of $1.28{\pm}0.19MPa{\cdot}m^{1/2}$ and Rosetta BM of $1.38{\pm}0.12MPa{\cdot}m^{1/2}$. The Rosetta BM sample exhibited higher strength and fracture toughness. Moreover, the crystalline phase size and ratio were increased in the Rosetta BM sample. The above results are expected to elucidate the basic mechanical properties and crystal structure characteristics of IPS Empress CAD and Rosetta BM. Additionally, they will help develop leucite-reinforced glass-ceramic materials for CAD/CAM.

• The Journal of Korean Academy of Prosthodontics
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• v.36 no.5
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• pp.772-785
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• 1998

This study was undertaken to clarify the microstructure of the different IPS Empress ingots by etching and to observe the change of leucite crystal structure according to subsequent heat treatment and the crystal distribution according to sprue types(${\phi}2.8mm$, single sprue; ${\phi}1.8mm$, double sprue) by scanning electron microscopy. IPS Empress T1, O1 ingots used for staining technique, and Dentin(A2) ingots used for layering technique were selected for this study. To observe the microstructures of these ingots before pressing, the specimens were prepared in splinters($3{\times}3{\times}3mm$) taken from the original ingots. And to estimate crystal distribution and microstructural change by sprue type and subsequent heat treatment. the specimens($3{\times}3{\times}3mm$) were heat-pressed through the two types of sprues with different diameters and numbers, and all specimens were fired according to the recommended firing schedule. The observed surface was ground with waterproof papers($#800{\sim}#1800$) on the grind polisher and was cleaned ultrasonically. All specimen were etched with 0.5% hydrofluoric acid. After etching, the surface was treated by ion sputter coating for SEM observation at an accelerating voltage of 20kV. In all specimens, the central area of ground surface was observed because there was less difference in microstructure between the peripheral area and the central area. The results were as follows ; 1. In the microstructure according to the ingot type, there was a wide difference between the staining (T1,O1) and layering(Dentin A2) ingots, but there was not a considerable difference between the T1 ingot and the O1 ingot for staining technique. 2. In all specimens, the crystal dispersion of IPS Empress ceramic using double sprue was significantly more scattered than that of IPS Empress ceramic using single sprue. The degree of scattering was strongest in the Dentin(A2) specimen and weakest in the O1 ingot. 3. In the microstructural change according to the subsequent heat treatment, all of ingots had some microcracks in the inside of the leucite crystal and the glass matrix after pressing. The inner splinters of the leucite crystal became smaller, and more microcracks occurred in the glass matrix due to increasing heat treatment times. 4. The size of leucite crystals varied from $1{\mu}m\;to\;5{\mu}m$. The mean size of mature crystals was about $5{\mu}m$. The form of the crystal was similar to a circle when it was smaller and similar to an ellipse when it was larger.

• The Journal of Korean Academy of Prosthodontics
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• v.41 no.5
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• pp.656-673
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• 2003

Statement of problem : Long-term exposure of dental porcelain to saliva during temporary cementation of a porcelain-fused to metal (PFM) restoration could affect mechanical strength of dental porcelain if the restoration is refired. Purpose : This work was performed to verify the effect of water on the mechanical strength in aged dental porcelain. Material and method : 63 specimens(Vintage Metalbond opaque and opal powder) were distributed to three experimental groups ; non-water immersed control, immersed and pedried, and immersed and non-predired groups. The changes in flexural strength and fracture toughness after specimen refiring related to Fourier Transform Infrared (FT-IR) spectroscopy. Results : 1. The FT-IR reflectances assigned to molecular bonds of $H_2O$ were noted as significantly different between the first-fired group and three refired groups and between two water-immersed groups and control group after refiring(p<0.05). They were also significantly different between predried group and non-predried group after refiring(p<0.05) 2. For opal specimens, FT-IR absorbances for hydrogen bond of $H_2O$ and silanols were significantly higher in non-predried group than in predreid group(p<0.05). 3 Predried opal group showed the highest mean flexural strength(p<0.05). Non-predried group indicated higher mean flexural strength than control group(p<0.05). 4. The mean fracture toughness for predired group was higher than non-predried group(p<0.05). 5. The difference of leucite crystal size is noted between control group and water-immersed, predried group in scanning electron microscopic study(${\times}10000$).

• Journal of the Korean Ceramic Society
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• v.41 no.2
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• pp.143-150
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• 2004

Biaxial flexure strength (ball-on-3-ball) and fracture toughness (indentation microfracture) of heat-pressable glass-ceramics for dental use were investigated in this study. Crystal phase and microstructure of glass-ceramics were analyzed by XRD. SEM, and TEM. Crack propagation in specimens was not effectively arrested by dispersed crystalline particles. However, higher degree of crystallization probably contributes to strengthening of glass-ceramics. Better clinical reliability can be expected from lithium disilicate glass-ceramic because of its significantly higher biaxial flexure strength and fracture toughness.

• Journal of the Korean Ceramic Society
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• v.31 no.10
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• pp.1218-1230
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• 1994

In manufacturing process of porous glass-ceramics by the filler method, the sintering behaviour of crystallizable glass powder mixed with various salts was studied and also the effects of precipitated crystal phases on the properties of porous glass-ceramics were investigated. Fine-grained crystallizable glass powder was homogeneously mixed with various slat having grain size 100~200 ${\mu}{\textrm}{m}$ and sintered for densification. After washing out the inorganic salt with distilled water, the porous sintered body was heat treated additionly for crystallization. The MgO-Al2O3-SiO2 base glass was used as crystallizable glass powder and the water soluble salts such as K2SO4 and MgSO4 were used as filler. When K2SO4 was used, leucite crystal phase was formed as a result of the ion exchange and porous glass-ceramics which exhibit high temperature resistance and high thermal expansion coefficient of 17$\times$10-6/$^{\circ}C$ could be obtained. On the contrary, when MgSO4 was used, only slight ion exchange is observed and $\mu$-cordierite and $\alpha$-cordierite crystal phases were formed and porous glass-ceramics which exhibit low thermal expansion coefficient schedule were determined with the results of DTA curves, thermal shrinkage curves and XRD patterns analysis. From DTA curves and thermal shrinkage curves, it was found that the sintering densification have been completed at the temperature range of exothermic peak for crystallization. The pore size distributions and pore diameters were measured by mercury porosimeter. The pore diameter of porous glass-ceramics was 10~15 ${\mu}{\textrm}{m}$ when 100~200${\mu}{\textrm}{m}$ grain size of K2SO4 was used and it was 25~30 ${\mu}{\textrm}{m}$ when the same grain size of MgSO4 was used. The porous glass-ceramics K2SO4 used shows bimodal pore size distribution and its porous skeleton structure was ascertained by SEM observation.