• Title/Summary/Keyword: Solid state sintering

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Structure and Magnetic Properties of Ho and Ni Co-doped BiFeO3 Ceramics

  • Hwang, J.S.;Yoo, Y.J.;Park, J.S.;Kang, J.H.;Lee, K.H.;Lee, B.W.;Kim, K.W.;Lee, Y.P.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.183-183
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    • 2014
  • Recently, multiferroic materials gain much attention due to their fascinating fundamental physical properties. These materials offer wide range of potential applications such as data storage, spintronic devices and sensors, where both electronic and magnetic polarizations can be coupled. Among single-phase multiferroic materials, $BiFeO_3$ is typical because of the room-temperature magnetoelectric coupling in view of long-range magnetic- and ferroelectric-ordering temperatures. However, $BiFeO_3$ is well known to have large leakage current and small spontaneous polarization due to the existence of oxygen vacancies and other defects. Furthermore the magnetic moment of pure $BiFeO_3$ is very weak owing to its antiferromagnetic nature. Recently, various attempts have been performed to improve the multiferroic properties of $BiFeO_3$ through the co-doping at the A and the B sites, by making use of the fact that the intrinsic polarization and magnetization are associated with the lone pair of $Bi^{3+}$ ions at the A sites and the partially-filled 3d orbitals of $Fe^{3+}$ ions at the B sites, respectively. In this study, $BiFeO_3$, $Bi_{0.9}Ho_{0.1}FeO_3$, $BiFe_{0.97}Ni_{0.03}O_3$ and $Bi_{0.9}Ho_{0.1}Fe_{0.97}Ni_{0.03}O_3$ bulk compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Ho_2O_3$, $Fe_2O_3$ and $NiO_2$ powders with the stoichiometric proportions were mixed, and calcined at $500^{\circ}C$ for 24 h to produce the samples. The samples were immediately put into an oven, which was heated up to $800^{\circ}C$ and sintered in air for 1 h. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The field-dependent and temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer and superconducting quantum-interference device.

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Photoluminescent Properties of $\textrm{Zn}_{2}\textrm{SiO}_{4}$: Mn Green Phosphors doped with Ga (Ga 도핑된 $\textrm{Zn}_{2}\textrm{SiO}_{4}$: Mn 녹색 형광체의 발광특성)

  • Park, Eung-Seok;Jang, Ho-Jeong;Jo, Tae-Hwan
    • Korean Journal of Materials Research
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    • v.8 no.9
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    • pp.860-864
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    • 1998
  • We investigated the photoluminescence and the crystalline properties with Ga doping concentrations (0-12 mol%) in $\textrm{Zn}_{1.98}\textrm{Mn}_{0.02}\textrm{SiO}_{4}$ green phosphors prepared by the solid state reaction. The photoluminescence was improved by a doping of Ga element in $\textrm{Zn}_{1.98}\textrm{Mn}_{0.02}(\textrm{Si_{1-x}\textrm{Ga}_{x})\textrm{O}_{4}$ phosphors which showed the highest emission intensity and good color purity in the doping concentration of x=0.08. The emission intensity of $\textrm{Zn}_{1.98}\textrm{Mn}_{0.02}(\textrm{Si_{1-x}\textrm{Ga}_{x})\textrm{O}_{4}$(x= 0.08) phosphors was increased to 7 times with increasing the sintering temperatures from $1100^{\circ}C$ to $1400^{\circ}C$, showing the improved crystalline quality. The decay time was not affected by Ga doping concentrations with constant values around 24ms. It was found from SEM and PSA analyses that the phosphors were composed of a large number of small grains around 1-3$10\mu\textrm{m}$ with a small amounts of agglomerated particles above $10\mu\textrm{m}$.

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Improved Physical Properties of Ni-doped $BiFeO_3$ Ceramic

  • Yoo, Y.J.;Park, J.S.;Kang, J.H.;Kim, J.;Lee, B.W.;Kim, K.W.;Lee, Y.P.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.250-250
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    • 2012
  • Recently, multiferroic materials have attracted much attention due to their fascinating fundamental physical properties and potential technological applications in magnetic/ferroelectric data storage systems, quantum electromagnets, spintronics, and sensor devices. Among single-phase multiferroic materials, $BiFeO_3$, in particular, has received considerable attention because of its very interesting magnetoelectric properties for application to spintronics. Enhanced ferromagnetism was found by Fe-site ion substitution with magnetic ions. In this study, $BiFe_{1-x}Ni_xO_3$ (x=0 and 0.05) bulk ceramic compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Fe_3O_4$ and NiO powders were mixed with the stoichiometric proportions, and calcined at $450^{\circ}C$ for 24 h to produce $BiFe_{1-x}Ni_xO_3$. Then, the samples were directly put into the oven, which was heated up to $800^{\circ}C$ and sintered in air for 20 min. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The Raman measurements were carried out with a Raman spectrometer with 514.5-nm-excitation Ar+-laser source under air ambient condition on a focused area of $1-{\mu}m$ diameter. The field-dependent magnetization and the temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer. The x-ray diffraction study demonstrates the compressive stress due to Ni substitution at the Fe site. $BiFe_{0.95}Ni_{0.05}O_3$ exhibits the rhombohedral perovskite structure R3c, similar to $BiFeO_3$. The lattice constant of $BiFe_{0.95}Ni_{0.05}O_3$ is smaller than of $BiFeO_3$ because of the smaller ionic radius of Ni3+ than that of Fe3+. The field-dependent magnetization of $BiFe_{0.95}Ni_{0.05}O_3$ exhibits a clear hysteresis loop at 300 K. The magnetic properties of $BiFe_{0.95}Ni_{0.05}O_3$ were improved at room temperature because of the existence of structurally compressive stress.

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Syntheses, Dielectric Properties and Ordering Structures of $Pb(Fe _{1/2}Ta_{1/2})O_3$ ($Pb(Fe _{1/2}Ta_{1/2})O_3$의 합성, 유전특성 및 질서배열구조)

  • 우병철;김병국;김병호
    • Korean Journal of Crystallography
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    • v.13 no.3_4
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    • pp.165-171
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    • 2002
  • Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$, ceramics were successfully synthesized from the powders prepared by solid state reaction (sintering temperature: $1100^{\circ}C$, density: $9.3g/cm^3$, average grain size: $5.1{\pm}1.2mm$, space group: Pm3m). Their dielectric properties measured at $-150{\sim}50^{\circ}C$ showed the maximum relative dielectric constant of 31000 at $-41^{\circ}C$. 1 kHz, and typical relaxor ferroelectrics characteristics such as diffuse phase transition and dielectric relaxation phenomena. However, the diffuseness of phase transition decreased and the dielectric properties became more normal ferroelectrics as the time of annealing at $1000^{\circ}C$ increased. By using Raman spectroscopy, it was revealed that the $Fe^{3+}$ and $Ta^{5+}$ ions in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, are stoichiometrically 1 : 1 ordered within the short-range that can not be probed even by transmission electron microscopy, and this stoichiometric 1 : 1 ordering is enhanced by the annealing. The relaxor ferroelectric characteristics in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, could be correlated with the stoichiometric 1 : 1 short-range ordering of B-site cations, and the decrease of relaxor ferroelectric characteristics in the annealed $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the enhanced stoichiometric 1 : 1 short-range ordering of B-site cations.

Preparation and Oxygen Permeability of Nb-doped BCFN Ceramic Membrane (Nb-doped BCFN 세라믹 막의 제조 및 산소투과 특성)

  • Kim, Jong-Pyo;Son, Sou-Hwan;Park, Jung-Hoon;Lee, Yong-Taek
    • Membrane Journal
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    • v.21 no.1
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    • pp.55-61
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    • 2011
  • $BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ oxide was synthesized by solid state reaction method. Dense ceramic membrane was prepared using as-prepared powder by pressing and sintering at $1,200^{\circ}C$. XRD result of membrane showed single perovskite structure. Leakage and oxygen permeation test were conducted on the membrane sealed by glass ring as a sealing material. The oxygen permeation flux increased with increasing temperature and pressure difference and maximum oxygen permeation flux was $2.3mL/min{\cdot}cm^2$ at $950^{\circ}C$ with $Po_2$ = 0.63 atm of oxygen partial pressure. The oxygen permeation in the condition of air with $CO_2$ (300 ppm) as feed stream decreased as much as only maximum 2.9% in comparison with air feed stream. It indicated $BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ membrane is more stable than another membrane for carbon dioxide.

High Luminance $Zn_2$$SiO_4$:Mn Phosphors for in PDP Application (고상법에 의한 PDP용 고휘도 $Zn_2$$SiO_4$:Mn 형광체 제조)

  • Jeon, Il-Un;Son, Gi-Seon;Jeong, Yang-Seon;Kim, Chang-Hae;Park, Hui-Dong
    • Korean Journal of Materials Research
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    • v.11 no.3
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    • pp.227-235
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    • 2001
  • In this work, Zn$_2$SiO$_4$:Mn phosphors were prepared by solid state reaction. The effect of sintering/reduction temperature, flow rate of H$_2$-5%/$N_2$-95% mix gas, and ball milling conditions have been investigated on the sake of PDP(Plasma Display Panel) application. The characteristics such as particle morphology and photoluminescence of prepared phosphors were compared to those of commercial Zn$_2$SiO$_4$:Mn Phosphors. It was found that the Phosphor synthesized at 130$0^{\circ}C$ with 0.08 Mn concentration had a maximum brightness, This brightness was increased more 20% by reduction treatment under 100me/min flow rate of 5%H$_2$-95%$N_2$ mixed gas. The size of particles decreased under 3$\mu\textrm{m}$ after ball milling. Especially, higher luminescence was obtained in our Zn$_2$SiO$_4$:Mn phosphors than commercial Zn$_2$SiO$_4$:Mn phosphors, so that they are able to be applied for PDP.

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Oxygen Permeability and Resistance to Carbon Dioxide of SrCo0.8Fe0.1Nb0.1O3-δ Ceramic Membrane (SrCo0.8Fe0.1Nb0.1O3-δ 세라믹 분리막의 산소투과 특성 및 이산화탄소에 대한 내성)

  • Kim, Eun Ju;Park, Se Hyoung;Park, Jung Hoon;Baek, Il Hyun
    • Membrane Journal
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    • v.25 no.5
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    • pp.415-421
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    • 2015
  • $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ oxide was synthesized by solid state reaction method. Dense ceramic membrane was prepared using as-prepared powder by pressing and sintering at $1250^{\circ}C$. XRD result of membrane showed single perovskite structure. The oxygen permeability were measured under 0.21 atm of oxygen partial pressure ($P_{O_2}$) and between 800 and $950^{\circ}C$. The oxygen permeation flux of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ membrane was increased with the increasing temperature. The maximum oxygen permeation flux was $1.839mL/min{\cdot}cm^2$ at $950^{\circ}C$. Long period permeability experiment was carried out to confirm the phase stability and $CO_2$-tolerance of membrane containing Nb in the condition of air with $CO_2$ (500 ppm) as feed stream at $900^{\circ}C$. The phase stability and $CO_2$-tolerance of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ were investigated by XRD and TG analysis. The result of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ which exposed carbon dioxide for 100 hours indicated 8wt% of $SrCO_3$. But it was known that the level of $SrCO_3$ production dose not have a significant effect on oxygen permeability.

The effect of Dy2O3 addition on crystal structure, grain growth, and dielectric properties in BaTiO3 (BaTiO3에서 Dy2O3 첨가가 결정구조, 입자성장 및 유전특성에 미치는 영향)

  • Ahn, Won-Gi;Choi, Moonhee;Kim, Minkee;Moon, Kyoung-Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.4
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    • pp.136-142
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    • 2022
  • The crystal structure, grain growth behavior, and dielectric properties of BaTiO3 have been studied with the addition of Dy2O3. The powders were synthesized at ratios of (100-x)BaTiO3-xDy2O3 (mol%, x = 0, 0.5, 1.0, 2.0) by a conventional solid-state synthesis, and the powder compacts were sintered at 1250℃ for 2 hours in air. As the amount of added Dy2O3 was increased, the crystal structure of the sintered samples changed from a tetragonal to a pseudo-cubic structure, and the tetragonality decreased. In addition, a secondary phase of Ba12Dy4.67Ti8O35 appeared when Dy2O3 was added. The average grain size after sintering decreased and abnormal grains appeared as the amount of Dy2O3 increased. It can be explained that the grain growth behavior of the Dy2O3 added-BaTiO3 occurs due to the two-dimensional nucleation and growth, and is governed by the interface reaction. Further, the correlation between crystal structure, microstructure, and dielectric properties was discussed.