• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.35 no.4
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• pp.407-411
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• 2022

Bulk-sized PbTiO₃ (PT), which is widely known as a high-performance ferroelectric oxide but cannot be fabricated into a monolithic ceramic due to its high c/a ratio, was successfully prepared with a high tetragonality by partially substituting Ni ions for Pb ions using a solid-state reaction method. We found that Ni-doped PT was well-fabricated as a bulk monolith with a significant c/a ratio of ~1.06. X-ray diffraction on as-sintered and crushed samples revealed that NiTiO₃ secondary phase was present at the doping level of more than 2 at.%. Scanning electron microscopic study showed that NiTiO₃ secondary phase grew on the surface of PT specimens regardless of the doping level possibly due to the evaporation of Pb during sintering. We demonstrated that an unconventional introduction of Ni ions into A-site plays a key role on the fabrication of bulk PT, though how Ni ion functions should be studied further. We expect that this study contributes to a further development of displacive ferroelectric oxides with a high c/a ratio.

• Nuclear Engineering and Technology
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• v.55 no.2
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• pp.575-579
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• 2023

In this work, pure W and W-0.5wt%HfC alloy (WHC05) were fabricated by sintering and hot-rolling following the same processing route. After exposing to a high flux deuterium plasma irradiation with the D⁺ flux to three fluences of 6.00 × 10²⁴, 2.70 × 10²⁵ and 7.02 × 10²⁵ D/m², the evolution of surface morphology, deuterium retention and hardening behaviors in pure W and WHC05 has been studied. The SEM results show the formation of D blisters on the irradiated area, and with the increase of D implantation, the size of these blisters increases from 200 ~ 500 nm (2.70 × 10²⁵ D/m²) to 1 ~ 2 ㎛ (7.02 × 10²⁵ D/m²) in WHC05 and from 1 ~ 2 ㎛ (2.70 × 10²⁵ D/m²) to > 3 ㎛ (7.02 × 10²⁵ D/m²) in pure W, respectively. A higher D retention and obvious hardening are observed in pure W than that of the WHC05 alloy, indicating an improve radiation resistance in WHC05 compared to pure W.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.6
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• pp.314-319
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• 2013

Fabrication of nanocomposite material for the $Fe_2O_3-Al$ system by mechanical alloying (MA) has been investigated at room temperature. It is found that ${\alpha}-Fe/Al_2O_3$ nanocomposite powders in which $Al_2O_3$ is dispersed in ${\alpha}-Fe$ matrix are obtained by mechanical alloying of $Fe_2O_3$ with Al for 5 hours. The change in magnetization and coercivity also reflects the details of the solid state reduction process of hematite by pure metal of Al during mechanical alloying. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $1000^{\circ}C$ and $1100^{\circ}C$ under 60 MPa. Shrinkage change after SPS of MA'ed sample for 5 hrs was significant above $700^{\circ}C$ and gradually increased with increasing temperature up to $1100^{\circ}C$. X-ray diffraction result shows that the average grain size of ${\alpha}-Fe$ in ${\alpha}-Fe/Al_2O_3$ nanocomposite sintered at $1100^{\circ}C$ is in the range of 180 nm. It can be also seen that the coercivity (Hc) of SPS sample sintered at $1000^{\circ}C$ is still high value of 88 Oe, suggesting that the grain growth of magnetic ${\alpha}-Fe$ phase during SPS process tend to be suppressed.

• Journal of the Korean Ceramic Society
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• v.39 no.10
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• pp.994-1000
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• 2002

Oxygen permeability and the mechanical properties of mixed ionic-electronic conductive $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-{\delta}}$ perovskite-type membrane, fabricated by solid state reaction, were investigated with regard to microstructure. The microstructure of the membrane was controlled by changing the sintering temperature and holding time. The average grain size and relative density were evaluated as a function of sintering conditions. As the fraction of grain boundary decreased, oxygen permeability showed a tendency to increase. Especially the maximum oxygen flux of 0.37 ml/$cm^2$${\cdot}$min was measured for the specimen sintered at 1300${\circ}C$ for 10 h, which has high density and relatively large grain size. Fracture strength was dependent on the relative density of sintered body, while fracture toughness increased with average grain size.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.24 no.7
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• pp.563-567
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• 2011

The most widely used piezoelectric ceramics are lead oxide based ferroelectrics (PZT). However, the toxicity of lead oxide and its high vapor pressure during processing have led to a demand for alternative lead-free piezoelectric materials. We synthesized Lead-free piezoelectric ceramics of $0.96(K_{0.5}Na_{0.5})NbO_3-0.04SrZrO_3+x$ mol% $ZrO_2$ [KNN-SZ+$xZrO_2$; x= 0~0.10] doped with 0.1 wt% $MnO_2$ by a conventional solid state method. We investigated the piezoelectric properties and microstructures of these disk samples sintered in reduced atmosphere in order to evaluate the possibility of the multilayered piezoelectric ceramics having the base metal such as Ni as a internal electrode. All of these KNN-SZ samples sintered in 3%$H_2-97%N_2$ atmosphere at $1,140^{\circ}C$ exhibit pure perovskite structure irrespective of the content of $ZrO_2$. Meanwhile, the sintering denisty and piezoelectric properties such as $K_p$, $Q_m$ and $d_{33}$ of KNN-SZ samples as a function of $ZrO_2$ content show the maxima ($k_p$=28.07%, $Q_m$= 101.34, $d_{33}$= 156 pC/N) at x= 0.04 and it is likely that there is some morphotropic phase boundary(MPB) in this KNN-SZ+$xZrO_2$ composition system. These results indicate that the ceramic composition is a promising candidate material for applications in lead free multilayer piezoelectric ceramics.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.1
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• pp.57-63
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• 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 the Korean Ceramic Society
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• v.45 no.11
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• pp.701-706
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• 2008

High frequency dielectric ceramics have potential for applications in mobile and satellite communications systems at frequencies higher than 10GHz. The Ba$(Zn_{1/3}Ta_{2/3})O_3$ ceramics are known to have a high quality factor, a small temperature coefficient of the resonance frequency and a high dielectric constant. On the other hands, sintering at high temperature for extended time is required to obtain the ordered structure for high quality factor. In this study, the microwave dielectric properties of $ZrO_2$ and NiO-added Ba$(Zn_{1/3}Ta_{2/3})O_3$ ceramics prepared by solid-state reaction have been investigated. Adding $ZrO_2$ and NiO could effectively promote the densification even the case of decreasing the sintering time. At the surface of samples, secondary phase of Ba-Ta compounds was formed possibly due to the evaporation of ZnO, however, the interior of the samples remained as pure Ba$(Zn_{1/3}Ta_{2/3})O_3$. The samples sintered at $1600^{\circ}C$ for 2h exhibited 1:2 ordering of Zn and Ta cations. Excellent microwave dielectric properties of $Q{\cdot}f$(>96,000 GHz) and ${\varepsilon}_r$=30 has been obtained.

• Journal of the Korean Electrochemical Society
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• v.24 no.3
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• pp.52-64
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• 2021

The effect of Fe and BO₃ doping on structure, thermal, and electrical properties of Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y (x = 0.2, 0.5)-based glass and glass ceramics was investigated. In addition, their crystallization behavior during sintering and ionic conductivity were also investigated in terms of sintering temperature. FT-IR and XPS results indicated that Fe²⁺ and Fe³⁺ ions in Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y glass worked as a network modifier (FeO₆ octahedra) and also as a network former (FeO₄ tetrahedra). In the case of the glass with low substitution of BO₃, boron formed (PB)O₄ network structure, while boron preferred BO₃ triangles or B₃O₃ boroxol rings with increasing the BO₃ content owing to boic oxide anomaly, which can result in an increased non-bridging oxygen. The glass transition temperature (GTT) and crystallization temperature (CT) was lowered as the BO₃ substitution was increased, while Fe²⁺ lowered the GTT and raised the CT. The ionic conductivity of Li_1+xFe_xTi_2-x(PO₄)_3-y(BO₃)_y glass ceramics were 8.85×10^-4 and 1.38×10^-4S/cm for x = 0.2 and 0.5, respectively. The oxidation state of doped Fe and boric oxide anomaly were due to the enhanced lithium ion conductivity of glass ceramics.

• Membrane Journal
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• v.22 no.2
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• pp.113-119
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• 2012

$YBaCo_2O_{5+{\delta}}$ oxide was synthesized by solid state reaction and a typical dense membrane has been prepared using as-prepared powder by unilateral pressing and sintering at $1,180^{\circ}C$. The $YBaCo_2O_{5+{\delta}}$ membraneswas analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM). XRD analysis showed the double layered perovskite structure was observed over $1,150^{\circ}C$ without impurities. Oxygen permeation was measured in the temperature range from 750 to $950^{\circ}C$ according to oxygen partial pressure difference between feed and permeation side. The oxygen permeation flux increased with increasing temperature and oxygen partial pressure and the maximum oxygen flux of $YBaCo_2O_{5+{\delta}}$ membrane with 1.0 mm thickness was about 0.15 mL/$cm^2{\cdot}min$ at $950^{\circ}C$ and $PO_2$ = 0.42 atm. The activation energy for oxygen permeation decreased with decreasing oxygen partial pressure to be 76.0 kJ/mol at the condition of $PO_2$ = 0.21 atm.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.260-260
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• 2013

Multiferroic materials have attracted much attention due to their fascinating fundamental physical properties and technological applications in magnetic/ferroelectric data-storage systems, quantum electromagnets, spintronics, and sensor devices. Among single-phase multiferroic materials, $BiFeO_3 $ is a typical multiferroic material with a room temperature magnetoelectric coupling in view of high magnetic-and ferroelectric-ordering temperatures (Neel temperature $T_N$~647 K and Curie temperature $T_C$~1,103 K). Rare-earth ion substitution at the Bi sties is very interesting, which induces suppressed volatility of Bi ion and improved ferroelectric properties. At the same time, Fe-site substitution with magnetic ions is also attracting, and the enhanced ferromagnetism was reported. In this study, $Bi_{1-x}Dy_xFe_{0.95}Co_{0.05}O_3$ (x=0, 0.05 and 0.1) bulk ceramic compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Dy_2O_3$, $Fe_2O_3$ and $Co_3O_4$ powders with the stoichiometric proportions were mixed, and calcined at $500^{\circ}C$ or 24 h to produce $Bi_{1-x}Dy_xFe_{0.95}Co_{0.05}O_3$. The samples were immediately put into an oven, which was heated up to $800^{\circ}C$ nd sintered in air for 30 min. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The field-dependent magnetization measurements were performed with a vibrating-sample magnetometer. The electric polarization was measured at room temperature by using a standard ferroelectric tester (RT66B, Radiant Technologies).