• Journal of the Korean Ceramic Society
• /
• v.26 no.1
• /
• pp.13-20
• /
• 1989

After sintering Si3N4 containing 20wt% of variable composition ratio of Y2O3 and Al2O3 at 1$600^{\circ}C$, the specimens were annealed at 125$0^{\circ}C$ and 135$0^{\circ}C$ for 5, 10, 15 hours in order to crystallize the remanining oxynitride glass phases. The main grain-boundary crystalline phases in the Si3N4-Y2O3-Al2O3 system were melilite and YAG. By annealing 15hrs. at 125$0^{\circ}C$, almost all of the glasses were crystallized. During the growth of melilite, lattice volyume of $\beta$-Si3N4 was increased as Al3+ and O2- ions in the oxynitride glass diffuse into $\beta$-Si3N4 lattice, but during the growth of YAG, lattice volume of $\beta$-Si3N4 was decreased by reverse diffusion of Al3+ and O2- ions. In case of crystallization of glass phase to melilite, thermal expansion of sample was decreased, but in case of crystallization to YAG, inverse phenomen on was observed.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 1997.11a
• /
• pp.39-43
• /
• 1997

Effects of B$_2$O$_3$ addition in the Li$_2$O-MgO-MgF$_2$-SiO$_2$g1ass system were investigated in order to make glass-ceramics for low temperature firing substrate. Base glass was made by melting at 145$0^{\circ}C$ . This glass was analyzed by THA and DTA to settle nucleation and crystallization temperature. After crystallization. crystal phase and microstructure were absorvated by XRD and SEM. Glass powders were made by water swelling method. Average particle size was 5.44${\mu}{\textrm}{m}$

• Journal of the Korean Ceramic Society
• /
• v.50 no.1
• /
• pp.70-74
• /
• 2013

Dependence of microwave dielectric properties on the crystallization behaviors of $CaMgSi_2O_6$ (diopside) glass-ceramics was investigated with different heat treatment methods (one and/or two-step). The crystallization behaviors of the specimens, crystallite size and degree of crystallization, were evaluated by differential thermal analysis (DTA), scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis by combined Rietveld and reference intensity ratio (RIR) methods. With an increase in heattreatment temperature, the dielectric constant (K) and the quality factor (Qf) increased due to the increase of the crystallite size and degree of crystallization. The specimens heat-treated by the two-step method had a higher degree of crystallization than the specimens heat-treated by the one-step method, which induced improvement in the quality factor (Qf) of the specimens.

• Journal of the Korean Ceramic Society
• /
• v.22 no.2
• /
• pp.44-50
• /
• 1985

The crystallization behavior of $K_2O-SiO_2$ glasses with added $TiO_2$ and the effect of $TiO_2$ on internal nuleation at temperature in the range of 875 to 121$0^{\circ}C$ have been investigated by means of X-ray diffractometry optical microscopy and scanning electron microscopy. The crystalline phase of these glasses identified by X-ray diffractometry is cristbalite. The scanning electron microspcopy reveals a two-phase layer of dendritic crystals and intersitial melt which grow from the surface at a constant rate, The observed crystallization rates are consistent with a diffusion-controlled mechanism. An equation relating viscosity and undercooling to growth rate is presented.

• 한국신재생에너지학회:학술대회논문집
• /
• 2010.06a
• /
• pp.59.1-59.1
• /
• 2010

Aluminum-induced crystallization (AIC) of amorphous silicon (a-Si) is studied with the structure of a glass/Al/$SiO_2$/a-Si, in which the $SiO_2$ layer has micron-sized laser holes in the stack. An oxide layer between aluminum and a-Si thin films plays a significant role in the metal-induced crystallization (MIC) process determining the properties such as grain size and preferential orientation. In our case, the crystallization of a-Si is carried out only through the key hole because the $SiO_2$ layer is substantially thick enough to prevent a-Si from contacting aluminum. The crystal growth is successfully realized toward the only vertical direction, resulting a crystalline silicon grain with a size of $3{\sim}4{\mu}m$ under the hole. Lateral growth seems to be not occurred. For the AIC experiment, the glass/Al/$SiO_2$/a-Si stacks were prepared where an Al layer was deposited on glass substrate by DC sputter, $SiO_2$ and a-Si films by PECVD method, respectively. Prior to the a-Si deposition, a $30{\times}30$ micron-sized hole array with a diameter of $1{\sim}2{\mu}m$ was fabricated utilizing the femtosecond laser pulses to induce the AIC process through the key holes and the prepared workpieces were annealed in a thermal chamber for 2 hours. After heat treatment, the surface morphology, grain size, and crystal orientation of the polycrystalline silicon (pc-Si) film were evaluated by scanning electron microscope, transmission electron microscope, and energy dispersive spectrometer. In conclusion, we observed that the vertical crystal growth was occurred in the case of the crystallization of a-Si with aluminum by the MIC process in a small area. The pc-Si grain grew under the key hole up to a size of $3{\sim}4{\mu}m$ with the workpiece.

• Journal of the Korean Society of Safety
• /
• v.14 no.1
• /
• pp.101-107
• /
• 1999

$TiO_2$ and $xTiO_2-ySiO_2$ system photocatalysts were developed by sol-gel method based on the change of production parameters, and their structure of crystallization and the specific surface area was measured. Considering the efficiency of the ethanol decomposition using the catalyst, the conclusion was made as follows: 1) By means of X-ray analysis of $TiO_2$ powder that is obtained from water and Titanium alkoxide with various molar ratios, it is shown that structure of crystallization is a dominating structure and, on the other hand, the crystallization of rutile also partly exists. The specific surface area is at its maximum value at R=6, which is the molar ratio of water vs. alkoxide, whereas its value goes down as the molar ratio increases. In the reaction of using $TiO_2$ catalyst, the ethanol is decomposed into the extent of 15 ~30% in an hour and three hours are necessitated for 70% decomposition. 2) $TiO_2/SiO_2$ powder is developed from Titanium and Silicon alkoxide by a hetero-condensation process. The increase of SiO$_2$ contents causes the decrease of the degree of crystallization of the gel, whereas the specific surface area preferentially increases. In the decomposition reaction of the ethanol, the decomposition efficiency represents 25~60% in an hour. It is, however, examined that the efficiency inactively increases corresponding to the duration of reaction time. It is shown that more than 90% of ethanol is decomposed when reaction time is about three hours and the efficiency illustrates the maximum value for 60-$TiO_2/4O-SiO_2$ catalyst.

• Journal of Industrial Technology
• /
• v.20 no.A
• /
• pp.247-256
• /
• 2000

Precursor gels with the composition of $xZrO_2{\cdot}(100-x)SiO_2$ systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence on tetragonal to monoclinic transformation of $ZrO_2$ was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal $ZrO_2$ occurred through 3-dimensional diffusion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about $310{\sim}325{\pm}10kJ/mol$. The growth of $t-ZrO_2$, in proportion to the cube of radius, increased with increasing heating temperature and heat-treatment time. It was suggested that the diffusion of Zr4+ions by Ostwald ripening was rate-limiting process for the growth of $t-ZrO_2$ crystallite size. The fracture toughness of $xZrO_2{\cdot}(100-x)SiO_2$ systems glass ceramics increased with increasing crystallite size of $t-ZrO_2$. The fracture toughness of $30ZrO_2{\cdot}70SiO_2$ system glass ceramics heated at $1,100^{\circ}C$ for 5 h was $4.84Mpam^{1/2}$ at a critical crystaliite size of 40 nm.

• Journal of the Korean Ceramic Society
• /
• v.48 no.4
• /
• pp.269-277
• /
• 2011

Glass-ceramics based on lithium disilicate($Li_2Si_2O_5$) are prepared by heat-treatment of glasses in a system of $SiO_2-Li_2O-K_2O-Al_2O_3$ with different compositions. The crystallization heat-treatment was conducted at the temperature range of $700{\sim}900^{\circ}C$ and samples were analyzed by XRD and SEM. Mechanical properties were determined by a Vicker's hardness and 4 point bending strength. When $SiO_2/Li_2O$ ratio increased, cristobalite and tridymite crystals showed more predominate than lithium disilicate crystals. Increase in $Al_2O_3$ contents in the glass suppressed crystallzation of lithium disilicate crystals. Increase in ZnO, $B_2O_3$ contents in the glass decreased crystallization temperature of lithium disilicate crystals, and increased mechanical properties because of the reduction of the lithium disilicate crystal size.

• Journal of the Korean Ceramic Society
• /
• v.27 no.4
• /
• pp.521-528
• /
• 1990

Li2O.2SiO2 glass-ceramics were made from the melt by the nucleation and growth treatment. The optimum nucleation temperature and time were determined from DTA curves of as-quenched and thermally treated glasses, and found to be 44$0^{\circ}C$ and 3hrs. The optical microscopic technique was also used to support this result. The volume fractions of crystals present in the partially crystallized specimens were measured using the optical microscopy and the amorphous X-ray scattering methods. The degree of crystallization increased with increasing the crystallization temperature and time. The crystalline phase identified by X-ray diffraction was lithium disilicate. As the crystallinity increased up to 95%, the transmittance of glass-ceramics was decreased linearly. It was also found that for the same heat treatment condition (575$^{\circ}C$, 30min), a thicker specimen showed higher transmittance, presumably due to less crystallinity.

• Journal of the Korean Ceramic Society
• /
• v.26 no.5
• /
• pp.705-711
• /
• 1989

The glass-ceramics was prepared with the scoria(CaO-MgO-Al2O3-SiO2 system) of the locally occurring volcanic ejecta containing 10-13w/o of (FeO＋Fe2O3) by melting at 140$0^{\circ}C$ for 4 hours and thermally treated for nucleation and crystallization. The sucrose was added to the scoria to adjust the Fe2+/Fe3+ ratio during the melting process. The addition of 1-2w/o of sucrose showed the glass-ceramics body with the finest particle developed and dispersed over the entire range. It is concluded that the impurity content of iron oxide and titanium oxide play the most-influencial effect on the crystallization. When 1-2w/o of sucrose was added to the scoria, the value of Fe2+/Fe3+ ratio was 0.93-1.32 and showed the best result of crystallization. The nucleation temperature and time were calculated by the measurements of exothermic peak temperatures of DTA for quenched and thermally treated glasses. The nucleation temperature of scoria glass without the addition of sucrose was estimated as 75$0^{\circ}C$, but the addition of sucrose by 2w/o showed the nucleation temperature 6$25^{\circ}C$. The nucleation time was calculated with the same DTA curves. The nucleation times estimated were about 150min. for both of glasses without and with sucrose added. Finally, the activation energies for crystallization were calculated with the DTA data. The calculated activation energies were 143 Kcal/mole for the glass without addition of sucrose and 90Kcal/mole, 87Kcal/mole, 85Kcal/mole and 71Kcal/mole for the glasses of 1w/o, 2w/o, 3w/o and 4w/o addition respectively.