• 한국분말재료학회지
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• 제20권6호
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• pp.405-410
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• 2013

During sintering of Ni-electrode multi-layer ceramic capacitors (MLCCs), the Ni electrode often becomes discontinuous because of its lower sintering temperature relative to that of $BaTiO_3$. In an attempt to retard the sintering of Ni, we introduced passivation of the Ni powder. To find the optimal passivation conditions, a thermogravimetric analysis (TGA) was conducted in air. After passivation at $250^{\circ}C$ for 11 h in air, a nickel oxide shell with a thickness of 4-5 nm was formed on nickel nanoparticles of 180 nm size. As anticipated, densification of the compacts of the passivated Ni/NiO core-shell powder was retarded: the starting temperature of densification increased from ${\sim}400^{\circ}C$ to ${\sim}600^{\circ}C$ in a $97N_2-3H_2$ (vol %) atmosphere. Grain growth was also retarded during sintering at temperatures of 750 and $1000^{\circ}C$. When the sintering atmosphere was changed from wet $99.93N_2-0.07H_2$ to wet $99.98N_2-0.02H_2$, the average grain size decreased at the same sintering temperature. The conductivity of the passivated powder sample sintered at $1150^{\circ}C$ for 8 h in wet $99.93N_2-0.07H_2$ was measured to be $3.9{\times}10^4S/cm$, which is comparable with that, $4.6{\times}10^4S/cm$, of the Ni powder compact without passivation. These results demonstrate that passivation of Ni is a viable means of retarding sintering of a Ni electrode and hence improving its continuity in the fabrication of $BaTiO_3$-based multi-layer ceramic capacitors.

• 한국분말재료학회지
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• 제9권4호
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• pp.273-279
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• 2002

In this study, the WC-10 wt.%Co nanopowders doped by grain growth inhibiter were produced by three different methods based on the spray conversion process. Agglomerated powders with homeogenous distribution of alloying elements and with internal particles of about 100-200 nm in diameter were synthesized. The microstructural changes and sintering behavior of hardmetal compacts were compared with doping method and sintering conditions. The microstructure of hardmetals was very sensitive to doping methods of inhibitor. Nanostructured WC-Co hardmetal powder compacts containing TaC/VC doped by chemical method instead of ball-milling shown superior sintering densification, and the microstructure maintained ultrafine scale with rounded WC particles.

• 한국세라믹학회지
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• 제49권6호
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• pp.485-492
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• 2012

Dense and single phase $BiFeO_3$ (BFO) ceramics were prepared using attrition milled calcined (coarse) powders of an average particle size of ${\approx}3{\mu}m$ by conventional sintering process. A relative density of ${\approx}96%$ with average grain size $7.3{\mu}m$ was obtained when the powder compacts were sintered at $850^{\circ}C$ even for a shorter duration of 10 min. In contrast, densification barely occurred at $800^{\circ}C$ for up to 12 h rather the microstruce showed the growth of abnormal grains. The grain growth behavior at different temperatures is discussed in terms of nonlinear growth rates with respect to the driving force. The sample sintered at $850^{\circ}C$ for 12 h showed enhanced electrical properties with leakage current density of $4{\times}10^{-7}A/cm^2$ at 1 kV/cm, remnant polarization $2P_r$ of $8{\mu}C/cm^2$ at 20 kV/cm, and minimal dissipation factor (tan ${\delta}$) of ~0.025 at $10^6$ Hz. These values are comparable to the previously reported values obtained using unconventional sintering techniques such as spark plasma sintering and rapid liquid phase sintering.

• 한국세라믹학회지
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• 제39권6호
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• pp.528-534
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• 2002

CaO ceramics were prepared by conventional sintering process and their hydration behaviors were evaluated by measuring weight increment on saturated water vapor pressure at ambient temperature. CaCO$_3$ and limestone were used as CaO source materials and $Al_2$O$_3$, MgO and SiO$_2$ were added as sintering agents. $Al_2$O$_3$ was a liquid phase sintering agent to increase densification and grain growth rates, whereas MgO and SiO$_2$, densification and grain growth inhibitors. Regardless of composition, all of the prepared CaO ceramics showed the improved hydration resistance as bulk density increased. Especially, when bulk density was more than 3.0 g/㎤, there was no weight increment after 120 h of hydration. Therefore, to decrease contact area between CaO and water vapor by increasing bulk density with the $Al_2$O$_3$ sintering additive was effective for the improvement of CaO hydration resistance.

• 한국세라믹학회지
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• 제33권1호
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• pp.83-91
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• 1996

Monolithic AlN and AlN-W composites were fabricated by pressure-less sintering at 190$0^{\circ}C$ under nitrogen atmosphere and the influences of tungsten phase on the microstructure and mechanical properties were investi-gated. In the fabrication of sintered specimen no additive was used. And monolithic AlN showed substantial grain growth and low relative density. AlN-W composites were fully densified and grain growths of matrix were inhibited. The densification behavior of composites were inferred to be achieved through the liquid phase sintering process such as particle-rearrangement and solutino-reprecipitation. Also the oxid phases which is expected to form liquid phases duringsintering process were detected by XRD analysis. As the tungsten volume content increases fracture strength was decreased and fracture toughness was increased. It was suppo-sed that the strength decrease of composites with tungsten content was due to existence of interface phases. The subcritical crack growth behavior was observed from the stress-strain curve of composites. The effect of the secondary phase and interface phases on toughness in crease were studied through observation of crack propagation path and the influence of residual stress on crack propagation was investigated by X-ray residual stress measurement. In the result of residual stress measurement the compressive stress of matrix in composi-test was increased with tungsten volume content and the compressive stress distribution of matrix must have contributed to the inhibition of crack propagation.

• 한국세라믹학회지
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• 제28권10호
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• pp.767-776
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• 1991

Effects of the additions of SiB4 as burnable poison to UO2 on the green density, densification, interdependence between density-grain growth and microstructure of sintered UO2 were studied. UO2 pellets were sintered in flowing hydrogen, at temperature 1200, 1350, 1500, and 168$0^{\circ}C$ for 3 hours and at 168$0^{\circ}C$ for 0, 1, 3, and 10 hours, respectively. Green densities were in the range of about 4.5~5.4 g/㎤, and decreased as the amount of SiB4 increased when green pellets were made by with use of a double action press at 1000 kg/$\textrm{cm}^2$. The density of sintered UO2 pellets was around 92~94% of the theoretical density and did not change significantly as the amount of SiB2 addition increased. However, the density of sintered pellets decreased with the increase in SiB4. The grain growth could be characterized in terms of two stages: Grain growth occurred with the increasing density in the first stage, whereas the second stage was characterized by the grain growth without increasing of density. A liquid phase was observed at grain boundaries and grain edges in the microstructure of sintered UO2 pellets with 5000 ppm and 10,000 ppm SiB4. This liquid, possible formed at about 168$0^{\circ}C$, did not enhance the shrinkage, but appeared to accelarate the grain growth. It seems that the second stage grain growth was due to the presence of pressurized insoluble trapped gas in isolated pores.

• 한국분말재료학회지
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• 제8권1호
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• pp.61-69
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• 2001

Spark-Plasma Sintering(SPS) is one of the new sintering methods which takes advantages both inconventional pressure sintering and electric current sintering. It is known that SPS is very effective for the densification of hard-to-sinter materials like refractory metals, intermetallic compounds, glass and ceramics without grain growth. However, a clear explanation for sintering mechanism and an experimental evidence for the formation of weak plasma during SPS are not given yet. In this study, fundamental study on sintering behavior and mechanism of SPS was investiged. For this study, various spherical Fe powders were prepared such as as-received, as-reduced, and as-oxidized and then sintered by SPS facility. In order to confirm the surface cleaning effect during SPS neck region and fracture surface of sintered body was observed and analyzed by SEM/EPMA. Densification behavior was analyzed from the data of deflection along the pressure axis. Some specimens were additionally produced by Hot Pressing and the results were compared with those of SPS.

• 한국세라믹학회지
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• 제27권2호
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• pp.169-178
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• 1990

The sintering characteristics of ZrO2 were analyzed in terms of pore microstructure and kinetics of pore elimination. The pore structue of the ZrO2 sample prepared from colloid suspension was characterized by three distinct types of pores ; intradomain, interdomain, and intergglomerate pores. Sintering data at 1600$^{\circ}C$ showed that pores larger than a certain critical size(∼3$\mu\textrm{m}$) were difficult to remove, and this was analyzed in terms of the interagglomerate pore formed from the suspension under the condition of low kinetic stability, that is, the stability ratio smaller than its critical value. A theoretical equation for densification rate was derived and was applied to the densification rate of the ZrO2 polycrystalline body containging both the matrix(the 1st-generation) pores and the interagglomerate (the 2nd-generation) pores under the condition of slow grain growth.

• 한국세라믹학회지
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• 제45권12호
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• pp.760-765
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• 2008

In this study, the effects of small amounts (${\leq}3\;mol%$) of Li doping on the sintering characteristics and electrochemical performance of $(ZrO_2)_{0.89}(ScO_{1.5})_{0.1}(CeO_2)_{0.01}$ (ScSZ) were investigated. By adding 3 mol% lithium, the densification temperature of ScSZ was reduced from the conventional temperature of $1400^{\circ}C$ to $1200^{\circ}C$. It was found that Li doping also led to changes in the Zr:Sc ratio at the grain boundaries. Correspondingly, the dispersion of lithium zirconia at the grain boundaries accelerated the growth of ScSZ grains and increased the grain boundary resistance at temperatures below $450^{\circ}C$. At elevated temperatures of $450{\sim}750^{\circ}C$, the electrical conductivity of the ScSZ after doping remained almost unchanged under air and reducing atmospheres. These results suggest that the addition of lithium is promising for use in low temperature co-firing of ScSZ-based components for intermediate temperature solid oxide fuel cells.

• 한국분말재료학회지
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• 제10권6호
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• pp.374-382
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• 2003

During the sintering of powder materials, many these are microstructural phenomena are caused by atomic diffusion. (1) neck formation and compact densification, (2) grain growth, i.e., growth of matrix grains and dispersed grains, (3) alloying or generation of compound, (4) generations of peculiar and hard layers near sintered compact surface, etc. The studies of the present author and co-workers on these phenomena which were carried out during 40 years are briefly introduced.