• Title/Summary/Keyword: Reaction-sintering

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Ferroelectric and Magnetic Properties of Dy and Co Co-Doped $BiFeO_3 $ Ceramics

  • Yu, Yeong-Jun;Park, Jeong-Su;Lee, Ju-Yeol;Gang, Ji-Hun;Lee, Gwang-Hun;Lee, Bo-Hwa;Kim, Gi-Won;Lee, Yeong-Baek
    • 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).

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Effect of Pressing Process on the High-Temperature Stability of Yttria-Stabilized Zirconia Ceramic Material in Molten Salt of CaCl2-CaF2-CaO (CaCl2-CaF2-CaO 용융염에서 YSZ 세라믹의 고온 안정성에 미치는 성형공정의 영향)

  • Kim, Wan-Bae;Kwon, Suk-Cheol;Cho, Soo-Haeng;Lee, Jong-Hyeon
    • Korean Journal of Materials Research
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    • v.30 no.4
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    • pp.176-183
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    • 2020
  • The high-temperature stability of YSZ specimens fabricated by die pressure and cold isostatic press (CIP) is investigated in CaCl2-CaF2-CaO molten salt at 1,150 ℃. The experimental results are as follows: green density 46.7 % and 50.9 %; sintering density 93.3 % and 99.3 % for die press and CIP, respectively. YSZ foremd by CIP exhibits higher stability than YSZ formed by die press due to denseness dependency after high-temperature stability test. YSZ shows peaks mainly attributed to CaZrO3, with a small t-ZrO2 peak, unlike the high-intensity tetragonal-ZrO2 (t-ZrO2) peak observed for the asreceived specimen. The t-ZrO2 phase of YSZ is likely stabilized by Y2O3, and the leaching of Y2O3 results in phase transformation from t-ZrO2 to m-ZrO2. CaZrO3 likely forms from the reaction between CaO and m-ZrO2. As the exposure time increases, more CaZrO3 is observed in the internal region of YSZ, which could be attributed to the inward diffusion of molten salt and outward diffusion of the stabilizer (Y2O3) through the pores. This results in greater susceptibility to phase transformation and CaZrO3 formation. To use SOM anodes for the electroreduction of various metals, YSZ stability must be improved by adjusting the high-density in the forming process.

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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A Study on the Preparation of Aluina & Titania Sols for Coatings (코팅용 알루미타, 티타니아솔 제조에 관한 연구)

  • Kim, Chu-Hui;Choe, Hyeong-Su;Jo, Yeong-Sang;Im, Jong-Ju
    • Korean Journal of Materials Research
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    • v.4 no.3
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    • pp.319-328
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    • 1994
  • Aluminium and titanium precursors containing $\beta$-diketonate ligands were used for the synthesis of polymeric sols of alumina and titania by sol-gel methods. To prepare polymeric sols by solgel processing, we synthesized modified precursors having chelating organic ligands. With these precursors it was found to be possible to control both hydrolysis and polycondensation reaction rates which resulted in ultrafine particles few nms of average size. The optimum molar ratio of acid to alkoxide for alumina sol was 0.3-0.4 and that of water to alkoxide &as 1. On the other hand, the corresponding ratios for titania sol were found be 0.25-0.20 and 1 respectively. Dynamic light scattering measurements indicated that the average particle size in both sols was in the order of few nms. SEM photographs were taken to observe crack-free and smooth surfaces of coated membranes after sintering at $450^{\circ}C$. Alumina coated membrane on a slide glass had about 4-4.5$\mu \textrm{m}$, thickness and titania coated one had 2-2.5$\mu \textrm{m}$, thickness. And according to TEM photographs, the grain size of titania was smaller than 30nm and that of alumina was in the range of few $\AA$s to 2nms. An X-ray diffraction study revealed that alumina was $\gamma$ phase and titania was anatase crystal.

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Catalytic Deep Oxidation of Volatile Organic Compounds Toluene and Toluene+Xylene over γPt/γ-Al2O3 Catalysts at Lower Temperatures (알루미나에 담지한 백금 촉매상에서 휘발성 유기화합물 톨루엔 및 톨루엔+자일렌의 저온산화)

  • Kim Sang-Hwan;Kang Tae-Sung;Yang Hee-Sung;Nhu Y Vu Trinh;Park Hyung-Sang
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.6
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    • pp.799-807
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    • 2006
  • The catalytic activity of $Pt/{\gamma}-Al_2O_3$ catalysts for the oxidation of toluene and toluene+xylene mixture was investigated in the microreactor of fixed-bed type. The calcination temperatures and loadings of $Pt/{\gamma}-Al_2O_3$ catalysts played the important role in the activity of catalysts for the oxidation of toluene. The increasing calcination temperatures and loadings of $Pt/{\gamma}-Al_2O_3$ catalysts increased the crystallite size of the platinum to result in the higher oxidation activity of catalysts. The catalytic activity for the toluene oxidation over $Pt/{\gamma}-Al_2O_3$ catalysts turned out to be increasing in the order of $500^{\circ}C\;<\;800^{\circ}C<600^{\circ}C\;<\;700^{\circ}C$ for calcination temperatures and 0.1 wt% < 0.3 wt% < 1.0 wt% for platinum loadings, respectively. The 1.0 wt% $Pt/{\gamma}-Al_2O_3$ catalysts calcined at $700^{\circ}C$ for 3 hrs in the air showed the highest activity for the oxidation of the toluene. The decrease of oxidation activity of $Pt/{\gamma}-Al_2O_3$ catalysts calcined at $800^{\circ}C$ might result from the decrease of active sites by sintering of platinum metals as well as ${\gamma}-Al_2O_3$ supports. The 1.0wt% $Pt/{\gamma}-Al_2O_3$ catalyst showed the activity from the lower temperature at $120^{\circ}C$, reached the light-off temperature ($T_{50%}$) at $180^{\circ}C$, and leveled off its activity at $340^{\circ}C$ with the conversion of 100% 'Mutual promotion' effects were observed for the binary mixture of toluene and xylene. The activity of the easy-to-oxidize toluene was slightly increased with the existence of the xylene. It might suggest the different mechanism for the oxidation of toluene and xylene on the $Pt/{\gamma}-Al_2O_3$ catalysts on different sites, and its reaction of gaseous oxygen.

Preparation of B4C-Al2O3 Composite Powder by Self-propagation High-temperature Synthesis(SHS) Process under High Pressure (고압 자전 고온반응 합성법에 의한 B4C-Al2O3복합분말 제조)

  • 임경란;강덕일;김창삼
    • Journal of the Korean Ceramic Society
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    • v.40 no.1
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    • pp.18-23
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    • 2003
  • Composite powder of$B_4C-A1_2O_3$was prepared from a mixed powder of$B_2O_3/A1/C$by SHS under argon pressure instead of using a chemical furnace. A mixture of$B_2O_3,$Al and C powder (equivalent amounts to the reaction,$2B_2O_3+4A1+C=B_4C+2A1_2O_3)$was ball milled for 2 h. The mixed powder was placed in a SHS reactor and filled with 10 atm of argon gas and ignited. The inner and outer products were the same by XRD analysis. It was consisted of a composite powder of$B_4C-A1_2O_3$without $AlB_{12}/C_2$which was always produced using a chemical furnace. The composite powder was about$60~100{mu}m$size which was composed of crystalline particles of about 0.3~l${mu}m$size. But when 15 atm of argon was employed, partial sintering took place to give rise hard composite powder of$15~25{mu}m$$B_4C$with $0.1~0.2{mu}m$$A1_2O_3.$

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.