• Title/Summary/Keyword: 고상소결법

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Synthesis and Luminescence Properties of $GdNbO_4$ : $Eu^{3+}$ Phosphors

  • Gwon, Bang-Gil;Jo, Sin-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.324-325
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    • 2011
  • 최근에 고효율의 적색 형광체를 합성하여 형광 램프, 음극선관, X-선 검출기, 전계 발광 디스플레이에 응용하기 위하여 다양한 모체 결정과 활성체를 도핑하는 연구가 활발히 진행되고 있다. 본 연구에서는 $GdNbO_4$ 모체 결정에 $Eu^{3+}$ 이온 활성체를 주입하여 합성함으로써 새로운 적색 형광체의 발광 세기와 입자의 형상을 최적화 시키고자 한다. 형광체 분말 시료의 제조는 Eu의 함량을 0, 0.05, 0.10, 0.15, 0.20 mol로 변화시키면서 고상 반응법을 이용하여 합성하였다. 초기 물질 Gd2O3 (99.99%), $Nb_2O_5$ (99.99%), $Eu_2O_3$ (99.9%)를 화학 적량으로 측량하고 에탄올과 ZrO2 볼과 함께 플라스틱 병에 넣어 400 rpm의 속도로 24시간 볼밀 작업을 수행한 후에, 혼합된 분말의 볼을 걸러내고 60$^{\circ}C$에서 20시간 동안 건조하였다. 건조된 시료를 막자 사발에 넣고 잘게 갈아서 체로 걸러낸 다음에 세라믹 도가니에 넣고 전기로에서 분당 5$^{\circ}C$씩 승온하여 500$^{\circ}C$에서 10시간 동안 1차 하소한 후에, 계속 온도를 승온시켜 1,200$^{\circ}C$에서 3시간 동안 소결하여 합성하였다. XRD 회절 패턴의 경우에, $Eu^{3+}$의 함량에 관계없이 모든 세라믹은 JCPDS (22-1104)에 제시된 회절상과 일치하는 사방정계의 결정 구조를 가짐을 확인할 수 있었다. 주 피크는 28.4$^{\circ}$에서 최대값을 갖는 (121)면에서 발생하는 회절 신호이었다(Fig. 1). 적색 형광체 분말의 광학 및 표면 특성은 PL, PLE와 SEM으로 조사되었으며, 세라믹 분말의 형광 특성과 결정 구조, 표면 형상에 대한 자세한 논의가 제시될 것이다.

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Sintering of Surface-Modified PMN-PT-BT Powder with MgO Sol and Its Dielectric Properties (MgO 졸로 표면개질된 PMN-PT-BT 분말의 소결 및 유전특성)

  • Han, Kyoung-Ran;Kim, Chang-Sam
    • Journal of the Korean Ceramic Society
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    • v.41 no.12 s.271
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    • pp.929-932
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    • 2004
  • It is known that small amount of MgO in excess is often added to develop pure perovskite single phase of PMN-based composite, however, extra MgO precipitates in grains and inhibits densification of PMN. In this study PMN-PT-BT (PBT) powder was prepared by a conventional mixed oxide method using $(MgCO_3)_4{\cdot}Mg(OH)_2{\cdot}5H_{2}O$ instead of MgO. The precursor was heated at $500^{\circ}C/1h$ and its surface was modified with MgO sol. This effect was investigated in the aspects of sintering and dielectric properties. Small amount of added MgO sol ($0.5{\sim}1.0wt\%$) enhanced sintering substantially below $1000^{\circ}C$. The PBT with $0.5wt\%$ MgO sol sintered at $900^{\circ}C/2h$ had density of $7.62\;g/cm^3$, room temperature dielectric constant of 14800, loss of dielectric constant of $1.1\%$, which were comparable to those of the PBT sintered at $1000^{\circ}C/2h$. It was noticeable that the extra MgO precipitated mostly on triple points and grain boundaries and resulted in inhibition of grain growth.

Preparation of $BaTiO_3$ powder in solid reaction and basic study on dielectrics of $CeAIO_3-BaTiO_3$system ($BaTiO_3$ 분말합성조건 및 $CeAIO_3-BaTiO_3$계 유전체의 기초적 연구)

  • Lim, Dae-Young;Kim, Jong-Ock;Lee, Chae-hyun;Park, Won-Kyu
    • The Journal of Natural Sciences
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    • v.8 no.1
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    • pp.61-69
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    • 1995
  • It is hard to synthesize pure $BaTiO_3$ from $BaCO_3$ and $TiO_2$ in solid reaction for the activity of BaO and secondary phase. For this reason, the wet chemical techniques have been studied. Starting material which was used in these methods were expensive and the properties of powder which was synthesized in same defined. So, some process have been studying again to improve soild reaction method. This study which was one of those was to defin the forming mechanism of $Ba_2TiO_4$ and to control some condition of $Ba_2TiO_4$. The synthesis temperature of $BaTiO_3$ in solid reaction was near $1120^{\circ}C$. The quantity and forming temperature of $Ba_2TiO_4$ could be controlled by atmosphere heat treatment. $Ba_2TiO_4$ was related to expansion in Ba-rich region of $BaTiO_3$. $BaTiO_2O_5$ and $BaTiO_3O_7$ was reason to expand in Ti-rich region. The dielectrics of $CeAIO_3$ which was synthesized and sintered in reduction atmosphere and $BaTiO_3$ system were affected by $CeO_2$ which was formed for the decomposition of $CeAIO_3$ heat treatment in air.

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Effect of Agglomeration of $Nb_20_5$ on Formation Reaction, Sintering and Dielectric Properties in$Pb(MG_{1/3}Nb_{2/3})O_3$ (원료분체 $Nb_20_5$의 응집상태가 $Pb(MG_{1/3}Nb_{2/3})O_3$소결, 유전특성에 미치는 영향)

  • 조영국;김진호;박병옥;조상희
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.2 no.1
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    • pp.51-59
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    • 1992
  • Effect of agglomeration of $Nb_20_5$ of the same primary particle size on formation reaction and sintering of $Pb(Mg_{1/3}\;Nb_{2/3})O_3$ was examined. Both solid state reaction and molten salt synthesis were adopted. With decreasing agglomeration of $Nb_20_5$ increased the rate of formation reaction of perovskite PMN in solid state reaction, but had little influence in molten salt synthesis. It was concluded that the increase in the inhomogeneity of the dispersion state of intermediate pyrochlore with increasing agglomeration of $Nb_20_5$ retarded the formation reaction of perovskite PMN in solid state reaction, while had little influnce in molten salt synthesis due to its solution - precipitation mechanism -mainly depends on powder surface area.

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Effect of Phase Stabilizers on the Phase Formation and Sintering Density of $Na^+$-Beta-Alumina Solid Electrolyte (상 안정화제가 $Na^+$-Beta-Alumina 고체 전해질의 상 형성 및 소결밀도에 미치는 영향)

  • Lee, Ki-Moon;Lee, Sung-Tae;Lee, Dae-Han;Lee, Sang-Min;Lim, Sung-Ki
    • Applied Chemistry for Engineering
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    • v.23 no.6
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    • pp.534-538
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    • 2012
  • $Na^+$-beta-alumina solid electrolyte was synthesized by solid state reaction using $Li_2O$ and MgO as a phase stabilizer, and the effect of stabilizers on the phase formation and sintering density was investigated. In order to determine the phase fraction according to the synthesizing temperature, the molar ratio of [$Na_2O$] : [$Al_2O_3$] was fixed at 1 : 5, and calcination was conducted at temperatures between $1200{\sim}1500^{\circ}C$ for 2 h. In the $Li_2O$-$Na_2O$-$Al_2O_3$ ternary system, ${\beta}^{{\prime}{\prime}}$-alumina phase fraction considerably increased by the secondary phase transition at $1500^{\circ}C$, whereas it maintained similarly in the MgO-$Na_2O$-$Al_2O_3$ system. Additionally, the disc-type specimens of $Na^+$-beta-alumina were sintered at the temperature between $1550{\sim}1650^{\circ}C$ for 30 min, and relative sintering densities, phase changes, and microstructures were analyzed. In case of $Li_2O$-stabilized $Na^+$-beta-alumina, ${\beta}^{{\prime}{\prime}}$-phase fraction and relative density of specimen sintered at $1600^{\circ}C$ were 94.7% and 98%, respectively. Relative density of MgO-stabilized $Na^+$-beta-alumina increased with a rise in sintering temperature.

Aerosol deposition method로 제작된 세라믹 후막 및 복합체 후막의 유전특성에 대한 연구

  • Jo, Seong-Hwan;Yun, Yeong-Jun;Kim, Hyeong-Jun;Kim, Hyo-Tae;Kim, Ji-Hun;Nam, Song-Min;Baek, Hong-Gu;Kim, Jong-Hui
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.311-311
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    • 2010
  • Aerosol deposition method(ADM)은 상온에서 에어로졸화 된 고상의 원료분말을 노즐을 통해 분사시켜 소결과정을 거치지 않고도 상온에서 고밀도 후막을 제조할 수 있는 공정이다. 이러한 Aerosol deposition method의 장점은 상온에서 고밀도 후막을 제조할 수 있고, 다양한 재료의 코팅이 가능하며, 코팅층의 조성 및 화학 양론비의 제어가 용이하다. 본 연구에서는 많은 장점을 가지고 있는 Aerosol deposition method를 이용하여 높은 유전상수, 압전계수, 초전계수를 갖는 $BaTiO_3$ 분말을 원료로 하여 압전소자, 커패시터, 고전압용 유전체 등에 응용이 가능한 유전체 형성에 관한 연구를 진행하였다. 또한 $BaTiO_3$ 같은 강유전체 세라믹을 이용하여 여러 가지 소자를 제조하는 경우 소자의 미세조직에 따라 물성이 영향을 받는 것으로 확인되어져 있다. 이에 본 연구에서는 세라믹 분말보다 상대적으로 탄성이 큰 polymer 분말 중 높은 유전율을 갖고 압전특성이 있는 Polyvinyl difluoride(PVDF)를 선정하여 $BaTiO_3$ 분말에 첨가하여 동시분사법을 사용해 복합체 후막을 성장시켰고, 또한 금속 분말을 첨가하여 동시분사법을 사용해 복합체 후막을 성장시켰다. 성장된 복합체 후막은 유전율과 유전손실 그리고 leakage current, breakdown voltage, 미세구조 분석 등 다양한 분석이 이루어 졌으며, embedded capacitor 유전체 층으로 응용 가능성을 가늠하였고, 상온에서 제조된 유전체 층의 응용을 위한 최적의 공정조건을 제시하고자 한다.

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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 Low-Voltage Luminescent Properties of $SrTiO_3$:Al, Pr Red Phosphor (저전압용 $SrTiO_3$ : Al, Pr 적색 형광체 합성 및 발광특성)

  • Park, Jeong-Gyu;Ryu, Ho-Jin;Park, Hui-Dong;Choi, Seung-Cheol
    • Korean Journal of Materials Research
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    • v.8 no.7
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    • pp.601-606
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    • 1998
  • The $SrTi0_3$:Al, Pr red phosphors were prepared by solid state reaction method. Phosphor preparation parameters such as sintering temperature and time were optimized for the photoluminescence(PU intensity and the cathodoluminescence(CL) intensity. Powder samples showed the characteristic X-ray diffraction patterns of the perovskite structure and the average particle size of 3~5/$\mu\textrm{m}$ for particle size distribution(PSD) analysis. Also, scanning electron microscopy for the powder samples showed that the particles are reasonably crystallized with spherical shape. Especially, higher low voltage CL properties of $SrTi0_3$:Al, Pr phosphors than commercial $Y_2O_3$:Eu phosphors are expected to be applied for a low voltage field emission display(FED).

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Oxygen Permeation Properties of $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-{\delta}}$ Mixed-conducting Membrane (혼합전도성 $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-{\delta}}$ 분리막의 산소투과 특성)

  • Lim, Kyoung-Tae;Cho, Tong-Lae;Lee, Kee-Sung;Woo, Sang-Kuk;Park, Kee-Bae;Kim, Jong-Won
    • Journal of the Korean Ceramic Society
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    • v.38 no.9
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    • pp.787-793
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    • 2001
  • $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_{3-{\delta}}$ membranes were fabricated by solid-state reaction. We investigated sintering behavior and oxygen permeation flux as a function of time-on-stream, temperature and upstream oxygen partial pressure. The oxygen was permeated at temperatures form 750$^{\circ}$C to 950$^{\circ}$C by mixed conducting through oxygen vacancy diffusion in the dense membrane. The oxygen permeation flux through the membrane were about 0.1ml/$cm^3{\cdot}$min at 850$^{\circ}$C. A constant time was required for reaching stable oxygen flux, and oxygen partial pressure affected the oxygen permeation fluxes.

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Optimization of anode and electrolyte microstructure for Solid Oxide Fuel Cells (고체산화물 연료전지 연료극 및 전해질 미세구조 최적화)

  • Noh, Jong Hyeok;Myung, Jae-ha
    • Korean Chemical Engineering Research
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    • v.57 no.4
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    • pp.525-530
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    • 2019
  • The performance and stability of solid oxide fuel cells (SOFCs) depend on the microstructure of the electrode and electrolyte. In anode, porosity and pore distribution affect the active site and fuel gas transfer. In an electrolyte, density and thickness determine the ohmic resistance. To optimizing these conditions, using costly method cannot be a suitable research plan for aiming at commercialization. To solve these drawbacks, we made high performance unit cells with low cost and highly efficient ceramic processes. We selected the NiO-YSZ cermet that is a commercial anode material and used facile methods like die pressing and dip coating process. The porosity of anode was controlled by the amount of carbon black (CB) pore former from 10 wt% to 20 wt% and final sintering temperature from $1350^{\circ}C$ to $1450^{\circ}C$. To achieve a dense thin film electrolyte, the thickness and microstructure of electrolyte were controlled by changing the YSZ loading (vol%) of the slurry from 1 vol% to 5 vol. From results, we achieved the 40% porosity that is well known as an optimum value in Ni-YSZ anode, by adding 15wt% of CB and sintering at $1350^{\circ}C$. YSZ electrolyte thickness was controllable from $2{\mu}m$ to $28{\mu}m$ and dense microstructure is formed at 3vol% of YSZ loading via dip coating process. Finally, a unit cell composed of Ni-YSZ anode with 40% porosity, YSZ electrolyte with a $22{\mu}m$ thickness and LSM-YSZ cathode had a maximum power density of $1.426Wcm^{-2}$ at $800^{\circ}C$.