• Journal of the Korean Ceramic Society
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• v.29 no.12
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• pp.935-941
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• 1992

The LAS system with good thermal properties has a narrow range of firing and sintering temperature near the melting point. So it is difficult to sinter LAS to dense sintered body. In this study, the petalite (Li2O.Al2O3.8SiO2) with good thermal properties, was taken as a base composition, and zironia was added in this composition to broaden the firing range, increase the mechanical strength, and control the thermal expansion. The thermal and mechanical properties were investigated. The results are as follows; 1. Zirconia phase was formed in LAS matrix and apparent porosity was decreased from 0.9% to 0.5%, and the mechanical strength was kincreased from 112 MPa to 190 MPa, by the densification of body. 2. The composition Li2O.Al2O3.8SiO2 has a negative thermal expansion, but the thermal expansion was changed from negative to positive with the densification and the increase of amount of synthesized zircon phase which had positive thermal expansion. The coefficient of thermal expansion, with the increase of the amount of additives, was low as -0.74~9.06$\times$10-7/$^{\circ}C$ in 20~$600^{\circ}C$, and 7.95~20.13$\times$10-7/$^{\circ}C$ in 20~80$0^{\circ}C$. 3. The mechanical strength of LZ15 (added with ZrO2.SiO2 15 wt%) composition thermal-shocked was stable in the temperature range of 0~$600^{\circ}C$, but rapidly decreased due to the increase of thermal expansion above $600^{\circ}C$.

• 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.

• Journal of Electrochemical Science and Technology
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• v.2 no.1
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• pp.39-44
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• 2011

Sub-micrometer $La_{0.8}Ca_{0.2}CrO_3$ powders for ceramic interconnects of solid oxide fuel cells were synthesized by the aqueous combustion process. The materials were prepared from the precursor solutions with different glycine (fuel)-to-nitrate (oxidant) ratios (${\phi}$). Single-phase $La_{0.8}Ca_{0.2}CrO_3$ powders with a perovskite structure were obtained after combustion when ${\phi}$ was equal to or larger than 0.480. Especially, the stoichiometric precursor with ${\phi}$ = 0.555 yielded the spherical $La_{0.8}Ca_{0.2}CrO_3$ particles with 150-250 nm diameters after calcination at $1000^{\circ}C$. When compared with the powders synthesized by the solid-state reaction, the combustion-derived, fine powders exhibited improved sinterability, leading to near-full densification at $1400^{\circ}C$ in oxidizing atmospheres. Moreover, a small quantity of glass additives was used to reduce the sintering temperature, and considerable densification was indeed achieved at temperatures as low as $1100^{\circ}C$.

• Journal of Powder Materials
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• v.30 no.5
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• pp.394-401
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• 2023

Li_1.5Al_0.5Ti_1.5(PO₄)₃ (LATP) is considered to be one of the promising solid-state electrolytes owing to its excellent chemical and thermal stability, wide potential range (~5.0 V), and high ionic conductivity (~10^-4 S/cm). LATP powders are typically prepared via the sol-gel method by adding and mixing nitrate or alkoxide precursors with chelating agents. Here, the thermal properties, crystallinity, density, particle size, and distribution of LATP powders based on chelating agents (citric acid, acetylacetone, EDTA) are compared to find the optimal conditions for densely sintered LATP with high purity. In addition, the three types of LATP powders are utilized to prepare sintered solid electrolytes and observe the microstructure changes during the sintering process. The pyrolysis onset temperature and crystallization temperature of the powder samples are in the order AC-LATP > CA-LATP > ED-LATP, and the LATP powder utilizing citric acid exhibits the highest purity, as no secondary phase other than LiTi₂PO₄ phase is observed. LATP with citric acid and acetylacetone has a value close to the theoretical density (2.8 g/cm³) after sintering. In comparison, LATP with EDTA has a low sintered density (2.2 g/cm³) because of the generation of many pores after sintering.

• Journal of the Korean Ceramic Society
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• v.30 no.5
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• pp.381-388
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• 1993

Due to the anisotropy of thermal expansion, LAS system which has low thermal expansion property is hard to obtain a dense sintered body. Therefore, the thermal expansion coefficient and the mechanical strength were decreased. In this study, mullite, which has good mechanical properties in high temperature and comparatively low thmeral expansion coefficient, was taken as a additive in LAS system. And then, sintering, thermal, and mechanical properties were investigated. The results are follows; When mullite is added in eucryptite composition (Li2O.Al2O3.2SiO2) of LAS system, the creation of liquid phase results in the densification of sintered body and the specimen sintered at 136$0^{\circ}C$ for 2 hours shows optimum sintering condition. With the addition of mullite in eucryptite composition, mechanical strength is increased by the control of grain growth. Especially, flexual strength of EM0 specimen was about double value than the basic composition. Thermal expansion coefficients of EM0 and EM15 specimens sintered at 136$0^{\circ}C$ were -8.23$\times$10-6/$^{\circ}C$ and -4.90$\times$10-6/$^{\circ}C$ in the temperature range of RT.~80$0^{\circ}C$. As the mullite content are increased, negative thermal expansion ratios are decreased.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.03a
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• pp.5-5
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• 2010

$(Na_{0.5}K_{0.5})NbO_3$ (NKN) ceramic with 1.5 mol% CuO added (NKNC) was well sintered even at a low temperature of $900^{\circ}C$ with the addition of ZnO. Most of the ZnO reacted with the CuO and formed the liquid phase that assisted the densification of the specimens at $900^{\circ}C$. A few $Zn^{2+}$ ions entered the matrix of the specimens and increased the coercive field ($E_c$) and $Q_m$ values of the specimens. High-piezoelectric properties of $k_p=0.37$, $Q_m=755$, and ${\varepsilon}_3\;^T/{\varepsilon}_0=327$ were obtained from the NKNC ceramics containing 1.0 mol% ZnO sintered at $900^{\circ}C$ for 2 h.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07a
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• pp.127-130
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• 2002

In this study, development of a new LTCC material using a non-glassy system was attempted with respect to reducing the fabrication process steps and cost down. Lowering the sintering temperature can be achieved by liquid phase sintering. For LTCC application, the starting material must have quality factor as high as possible in microwave frequency range. And also, the material should have a low dielectric constant for enhancing the signal propagation speed. Regarding these factors, dielectric constants of various materials were estimated by the Clausius-Mosotti equation. Among them, CaWO$_4$ was tamed out the suitable LTCC material. CaWO$_4$ can be sintered up to 98% of full density at 1200$^{\circ}C$ for 3 hours. It's measured dielectric constant, quality factor, and temperature coefficient of resonant frequency were 10.15, 62880GHz, and -27.8ppm/$^{\circ}C$, respectively. In order to modify the dielectric properties and densification temperature, 0.5∼1.5 wt% LiF were added to CaWO$_4$. LiF addition reduced the sintering temperature/time down to 800$^{\circ}C$/10∼30min due to the reactive liquid phase sintering. Dielectric constant lowered from 10.15 to 9.38 and Q x fo increased up to 92000GHz with increasing LiF content.

• Journal of the Korean Ceramic Society
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• v.56 no.1
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• pp.91-97
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• 2019

The effect of different Ni-containing additives on the sintering behavior and electric conductivity of the proton conducting electrolyte $BaCe_{0.35}Zr_{0.5}Y_{0.15}O_{3-{\delta}}$ (BCZY5) was investigated. Ni-doped, NiO-added, and $BaY_2NiO_5$(BYN)-added (all 4 mol%) BCZY5 samples were prepared by the solid state synthesis method and sintered at $1400^{\circ}C$ for 6 h. Among the three samples, the onset of densification was observed at the lowest temperature for NiO-added BCZY5, which is attributed to the formation of an intermediate phase at a low melting temperature. The BYN-added sample, where no consumption of the constitutional elements of the electrolyte was expected during sintering, exhibited the highest electrical conductivity whereas the doped sample had the lowest conductivity. The electrical conductivities at $500^{\circ}C$ under humid argon atmosphere were measured to be 2.0, 4.8, and $6.2mS{\cdot}cm^{-1}$ for Ni-doped and NiO- and BYN-added samples, respectively.

• Korean Journal of Mineralogy and Petrology
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• v.35 no.1
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• pp.65-73
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• 2022

The proper estimation of physical and chemical properties of Earth materials and their structures at high pressure and high temperature conditions is key to the full understanding of diverse geological processes in Earth and planetary interiors. Multi-anvil press - high-pressure generating device - provides unique information of Earth materials under compression, mainly relevant to Earth's upper mantle. The quantitative estimation of the relationship between the oil load within press and the actual pressure conditions within the sample needs to be established to infer the planetary processes. Such pressure-load calibration has often been based on the phase transitions of crystalline earth materials with known pressure conditions; however, unlike at high temperature conditions, phase transitions at low (or room) temperatures can be sluggish, making the calibration at such conditions challenging. In this study, we explored the changes in Al coordination environments of permanently densified pyrope glasses upon the cold compression using the high-resolution ²⁷Al MAS and 3QMAS NMR. The fractions of highly coordinated Al in the cold compressed pyrope glasses increase with increasing oil load and thus, the peak pressure condition. Based on known relationship between the peak pressure and the Al coordination environment in the compressed pyrope glasses at room temperature, we established a room temperature pressure-load calibration of the 14/8 HT assembly in 1,100-ton multi-anvil press. The current results highlight the first pressure-load calibration of any high pressure device using high-resolution NMR. Irreversible structural densification upon cold compression observed for the pyrope glasses provides insights into the deformation and densification mechanisms of amorphous earth materials at low temperature and high pressure conditions within the subducting slabs.

• Korean Journal of Materials Research
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• v.19 no.12
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• pp.680-685
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• 2009

Using a polyurethane foam replica method, porous hydroxyapatite scaffolds (PHS) were fabricated using conventional and microwave sintering techniques. The microstructure and material properties of the PHS, such as pore size, grain size, relative density and compressive strength, were investigated at different sintering temperatures and holding times to determine the optimal sintering conditions. There were interconnected pores whose sizes ranged between about 300 ${\mu}m$ and 700 ${\mu}m$. At a conventional sintering temperature of 1100$^{\circ}C$, the scaffold had a porous microstructure, which became denser and saw the occurrence of grain growth when the temperature was increased up to 1300$^{\circ}C$. In the case of microwave sintering, even at low sintering temperature and short holding time the microstructure was much denser and had smaller grains. As the holding time of the microwave sintering was increased, higher densification was observed and also the relative density and compressive strength increased. The compressive strength values of PHS were 2.3MPa and 1.8MPa when conventional and microwave sintering was applied at 1300$^{\circ}C$, respectively.