• Title/Summary/Keyword: Solid state synthesis

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Effect of Nickel Addition on Sintering Behavior and Electrical Conductivity of BaCe0.35Zr0.5Y0.15O3-δ

  • An, Hyegsoon;Shin, Dongwook;Ji, Ho-Il
    • Journal of the Korean Ceramic Society
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    • v.56 no.1
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    • pp.91-97
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    • 2019
  • The effect of different Ni-containing additives on the sintering behavior and electric conductivity of the proton conducting electrolyte $BaCe_{0.35}Zr_{0.5}Y_{0.15}O_{3-{\delta}}$ (BCZY5) was investigated. Ni-doped, NiO-added, and $BaY_2NiO_5$(BYN)-added (all 4 mol%) BCZY5 samples were prepared by the solid state synthesis method and sintered at $1400^{\circ}C$ for 6 h. Among the three samples, the onset of densification was observed at the lowest temperature for NiO-added BCZY5, which is attributed to the formation of an intermediate phase at a low melting temperature. The BYN-added sample, where no consumption of the constitutional elements of the electrolyte was expected during sintering, exhibited the highest electrical conductivity whereas the doped sample had the lowest conductivity. The electrical conductivities at $500^{\circ}C$ under humid argon atmosphere were measured to be 2.0, 4.8, and $6.2mS{\cdot}cm^{-1}$ for Ni-doped and NiO- and BYN-added samples, respectively.

Preparation of lead-free piezoelectric (K0.5Na0.5)NbO3 nanopowder by a simple aqueous route

  • John G. Fisher;Kwi-Hak Lee;Won-Jin Moon
    • Journal of Ceramic Processing Research
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    • v.21 no.1
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    • pp.5-13
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    • 2020
  • (K0.5Na0.5)NbO3-based ceramic powders for lead-free piezoelectric applications are usually prepared by solid state synthesis. This generally involves wet ball milling in an organic liquid such as ethanol, which is a drawback for industrial production. In the present work, a method for the preparation of NaNbO3 nanopowders is modified to produce a simple method of preparing (K0.5Na0.5)NbO3 nanopowders by an aqueous route. K2CO3, Na2CO3 and NH4[NbO(C2O4)2].xH2O are mixed in water and dried to form a gel, which is then calcined at temperatures between 400 ~ 650 ℃ for 1 h. The uncalcined gel and calcination products are analysed using Thermogravimetric Analysis/Differential Thermal Analysis, X-ray Diffraction, Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, Transmission Electron Microscopy and Raman Scattering. A single phase tetragonal (K0.5Na0.5)NbO3 nanopowder with a particle size of ~ 30 nm can be produced after calcination at 650 ℃ for 1 h.

Synthesis and Spectroscopic Characterization of Vanadium-Incorporated V-AlMCM-48 Mesoporous Material (바나듐이 들어있는 Mesoporous V-AlMCM-48 분자체의 합성 및 분광학적 특성 조사)

  • Back, Gernho;Yu, Jong-Sung;Park, Sung-Kun;Lee, Chul Wee;Won, Taejin
    • Korean Chemical Engineering Research
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    • v.44 no.4
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    • pp.369-374
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    • 2006
  • A solid-state reaction of $V_2O_5$ with AlMCM-48 followed by calcination generated very weak paramagnetic $VO^{2+}$ species in the mesoporous material. Dehydration and subsequent reduction with CO result in the formation of vanadyl $VO^{2+}$ species that can be characterized by EPR. The chemical environment of vanadium centers in $VO^{2+}-AlMCM-48$ was investigated by XRD, EDX, DR-UV-Vis, EPR,$^{29}Si$ and $^{27}Al$ and $^{51}V$ NMR. Vanadium species in MCM-48 are existed as pseudotetrahedral $VO^{2+}$ state when they were dehydrated or reduced with CO. The coordination of water on vanadyl ions transformed their structure to distorted octahedral.

Oxygen Permeation and Hydrogen Production of BaCo1-x-yFexZryO3-δ by a Modified Glycine-nitrate Process (MGNP) (Modified glycine-nitrate process(MGNP)로 합성한 BaCo1-x-yFexZryO3-δ 산소투과도 및 수소생산성)

  • Yi, Eunjeong;Hwang, Haejin
    • Journal of Hydrogen and New Energy
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    • v.24 no.1
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    • pp.29-35
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    • 2013
  • A dense mixed ionic and electronic conducting ceramic membrane is one of the most promising materials because it can be used for separation of oxygen from the mixture gas. The $ABO_3$ perovskite structure shows high chemical stability at high temperatures under reduction and oxidation atmospheres. $BaCo_{1-x-y}Fe_xZr_yO_{3-{\delta}}$ (BCFZ) was well-known material as high mechanical strength, low thermal conductivity and stability in the high valence state. Glycine Nitrate Process (GNP) is rapid and effective method for powder synthesis using glycine as a fuel and show higher product crystallinity compared to solid state reaction and citrate-EDTA method. BCFZ was fabricated by modified glycine nitrate process. In order to control the burn-up reaction, $NH_4NO_3$ was used as extra nitrate. According to X-Ray Diffraction (XRD) results, BCFZ was single phase regardless of Zr dopants from y=0.1 to 0.3 on B sites. The green compacts were sintered at $1200^{\circ}C$ for 2 hours. Oxygen permeability, methane partial oxidation rate and hydrogen production ability of the membranes were characterized by using Micro Gas Chromatography (Micro GC) under various condition. The high oxygen permeation flux of BCFZ 1-451 was about $1ml{\cdot}cm^{-2}s^{-1}$. Using the humidified Argon gas, BCFZ 1-433 produced hydrogen about $1ml{\cdot}cm^{-2}s^{-1}$.

Synthesis and Application of Bluish-Green BaSi2O2N2:Eu2+ Phosphor for White LEDs (백색 LED용 청록색 BaSi2O2N2:Eu2+ 형광체의 합성 및 응용)

  • Jee, Soon-Duk;Choi, Kang-Sik;Choi, Kyoung-Jae;Kim, Chang-Hae
    • Korean Journal of Materials Research
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    • v.21 no.5
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    • pp.250-254
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    • 2011
  • We have synthesized bluish-green, highly-efficient $BaSi_2O_2N_2:Eu^{2+}$ and $(Ba,Sr)Si_2O_2N_2:Eu^{2+}$ phosphors through a conventional solid state reaction method using metal carbonate, $Si_3N_4$, and $Eu_2O_3$ as raw materials. The X-ray diffraction (XRD) pattern of these phosphors revealed that a $BaSi_2O_2N_2$ single phase was obtained. The excitation and emission spectra showed typical broadband excitation and emission resulting from the 5d to 4f transition of $Eu^{2+}$. These phosphors absorb blue light at around 450 nm and emit bluish-green luminescence, with a peak wavelength at around 495 nm. From the results of an experiment involving Eu concentration quenching, the relative PL intensity was reduced dramatically for Eu = 0.033. A small substitution of Sr in place of Ba increased the relative emission intensity of the phosphor. We prepared several white LEDs through a combination of $BaSi_2O_2N_2:Eu^{2+}$, YAG:$Ce^{3+}$, and silicone resin with a blue InGaN-based LED. In the case of only the YAG:$Ce^{3+}$-converted LED, the color rendering index was 73.4 and the efficiency was 127 lm/W. In contrast, in the YAG:$Ce^{3+}$ and $BaSi_2O_2N_2:Eu^{2+}$-converted LED, two distinct emission bands from InGaN (450 nm) and the two phosphors (475-750 nm) are observed, and combine to give a spectrum that appears white to the naked eye. The range of the color rendering index and the efficiency were 79.7-81.2 and 117-128 lm/W, respectively. The increased values of the color rendering index indicate that the two phosphor-converted LEDs have improved bluish-green emission compared to the YAG:Ce-converted LED. As such, the $BaSi_2O_2N_2:Eu^{2+}$ phosphor is applicable to white high-rendered LEDs for solid state lighting.

Synthesis of Cathode Materials LiNi1-yCoyO2 from Various Starting Materials and their Electrochemical Properties

  • Song, Myoung-Youp;Rim, Ho;Bang, Eui-Yong;Kang, Seong-Gu;Chang, Soon-Ho
    • Journal of the Korean Ceramic Society
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    • v.40 no.6
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    • pp.507-512
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    • 2003
  • The LiN $i_{l-y}$ $Co_{y}$ $O_2$ samples were synthesized at 80$0^{\circ}C$ and 85$0^{\circ}C$, by the solid-state reaction method, from the various starting materials LiOH, L $i_2$C $O_3$, NiO, NiC $O_3$, $Co_3$ $O_4$, CoC $O_3$, and their electrochemical properties are investigated. The LiN $i_{l-y}$ $Co_{y}$ $O_2$ pre-pared from L $i_2$C $O_3$, NiO, and $Co_3$ $O_4$ exhibited the $\alpha$-NaFe $O_2$ structure of the rhombohedral system (space group; R3m). As the Co content increased, the lattice parameters a and c decreased. The reason is that the radius of Co ion is smaller than that of Ni ion. The increase in da shows that two-dimensional structure develops better as the Co content increases. The LiN $i_{0.7}$ $Co_{03}$. $O_2$[HOO(800,0.3)] synthesized at 80$0^{\circ}C$from LiOH, NiO, and $Co_3$ $O_4$ exhibited the largest first discharge capacity 162 mAh/g. The size of particles increases roughly as the valve of y increases. The samples with the larger particles have the larger first discharge capacities. The cycling performances of the samples with the first discharge capacity larger than 150 mAh/g were investigated. The LiN $i_{0.9}$ $Co_{0.1}$ $O_2$[COO(850,0.1)] synthesized at 85$0^{\circ}C$ from L $i_2$C $O_3$, NiO, and $Co_3$ $O_4$ showed an excellent cycling performance. The sample with the larger first discharge capacity will be under the more severe lattice destruction, due to the expansion and contraction of the lattice during intercalation and deintercalation, than the sample with the smaller first discharge capacity. As the first discharge capacity increases, the capacity fading rate thus increases.increases.s.s.s.

Fabrication of Gd1.5Ba2Cu3O7-y Bulk Superconductors from the Powder Synthesized by a Solid-State Reaction Method (고상반응법으로 합성한 분말로부터 Gd1.5Ba2Cu3O7-y 벌크 초전도체의 제조)

  • Kim, Yong Ju;Park, Seung Yeon;You, Byung Youn;Park, Soon-Dong;Kim, Chan-Joong
    • Korean Journal of Materials Research
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    • v.23 no.6
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    • pp.309-315
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    • 2013
  • $GdBa_2Cu_3O_{7-y}$(Gd123) powders were synthesized by the solid-state reaction method using $Gd_2O_3$ (99.9% purity), $BaCO_3$ (99.75%) and CuO (99.9%) powders. The synthesized Gd123 powder and the Gd123 powder with $Gd_2O_3$ addition ($Gd_{1.5}Ba_2Cu_3O_{7-y}$(Gd1.5)) were used as raw powders for the fabrication of Gd123 bulk superconductors. The Gd123 and Gd1.5 bulk superconductors were fabricated by sintering or a top-seeded melt growth (TSMG) process. The superconducting transition temperature ($T_{c,onset}$) of the sintered Gd123 was 93 K and the transition width was as large as 20 K. The $T_{c,onset}$ of the TSMG processed Gd123 was 82 K and the transition width was also as large as 12 K. The critical current density ($J_c$) at 77 K and 0 T of the sintered Gd123 and TSMG processed Gd123 were as low as a few hundreds A/$cm^2$. The addition of 0.25 mole $Gd_2O_3$ and 1 wt.% $CeO_2$ to Gd123 enhanced the $T_c$, $J_c$ and magnetic flux density (H) of the TSMG processed Gd123 sample owing to the formation of the superconducting phase with high flux pinning capability. The $T_c$ of the TSMG processed Gd1.5 was 92 K and the transition width was 1 K. The $J_cs$ at 77 K (0 T and 2 T) were $3.2{\times}10^4\;A/cm^2$ and $2.5{\times}10^4\;A/cm^2$, respectively. The H at 77 K of the TSMG-processed Gd1.5 was 1.96 kG, which is 54% of the applied magnetic field (3.45 kG).

Synthesis and Optical Properties of CaMoO4:RE3+ (RE=Eu, Dy) Phosphors (CaMoO4:RE3+ (RE=Eu, Dy) 형광체의 제조와 광학 특성)

  • Cho, Shinho
    • Journal of the Korean Vacuum Society
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    • v.22 no.2
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    • pp.79-85
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    • 2013
  • Rare earth ions, either $Eu^{3+}$ or $Dy^{3+}$-doped $CaMoO_4$ phosphors were synthesized by using the solid-state reaction method. The crystalline structure of all the phosphor powders, irrespective of the type and concentration of activator ions, was found to be a tetragonal system with the main diffraction peak at (112) plane. For $Eu^{3+}$-doped $CaMoO_4$ phosphors, the grain particles showed an increasing tendency and the pebble-like patterns with a very homogeneous size distribution in the range of 0.01~0.10 mol of $Eu^{3+}$ ions concentration, and the excitation spectra were composed of a broad band centered at 311 nm and weak multiline peaked in the range of 360~470 nm. The dominant emission spectrum was the strong red emission centered at 618 nm due to the $^5D_0{\rightarrow}^7F_2$ transition of $Eu^{3+}$ ions. For $Dy^{3+}$-doped $CaMoO_4$ powders, excitation spectra showed a charge transfer band centered at 303 nm and relatively weak bands resulting from the transitions of $Dy^{3+}$ ions and the main yellow emission spectrum was observed at 578 nm, which was assigned to the $^4F_{9/2}{\rightarrow}^7H_{13/2}$ transition of $Dy^{3+}$ ions.

Characterization and synthesis of aqueous pink-red ceramic ink for digital inkjet printing (잉크젯 프린팅용 pink-red 수계 무기잉크의 제조 및 특성평가)

  • Lee, Won-Jun;Hwang, Hae-Jin;Han, Kyu-Sung;Cho, Woo-Suk;Kim, Jin-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.1
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    • pp.20-26
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    • 2015
  • Ceramic ink-jet printing technology in art tiles, decorated tablewares and other porcelain products has many advantages of fast and precision printing of various images with high efficiency and low cost. For the application to ink-jet printing, ceramic ink requires a stable dispersibility with nano-sized pigments. In this paper, characteristics of pink-red aqueous ceramic ink for ink-jet printing was demonstrated. $CaCr_{0.1}Sn_{0.8}SiO_5$ pigment was synthesized using solid state reaction and deagglomerated using attrition milling. The aqueous ceramic ink contains 10 wt% of the obtained $CaCr_{0.1}Sn_{0.8}SiO_5$ nanopigment with 0.4 wt% of sodium dodecyl sulfate (SDS) as a dispersion agent. Viscosity of $CaCr_{0.1}Sn_{0.8}SiO_5$ aqueous ceramic ink was adjusted using 0.18 wt% of polyvinyl alcohol (PVA) for a suitable jetting from the nozzle. The prepared pink-red ceramic ink showed a good jetting property with formation of a single sphere-shaped droplet after $180{\mu}s$ without a tail and satellite droplet.

Synthesis and Emission Properties of Dy3+-doped BaMoO4 Phosphors (Dy3+ 이온이 도핑된 BaMoO4 형광체의 합성과 발광 특성)

  • Cho, Shinho
    • Journal of the Korean Vacuum Society
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    • v.22 no.4
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    • pp.181-187
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    • 2013
  • $Dy^{3+}$-doped $BaMoO_4$ phosphor powders were synthesized by using the solid-state reaction method and their crystalline structure, morphology and size of particles, excitation and emission properties were investigated. The structure of all the phosphor powders, irrespective of the mol ratio of $Dy^{3+}$ ions, was found to be the tetragonal system with the main diffraction peak at (112) plane. The grain particles agglomerate together to form larger clusters with increasing the mol ratio of $Dy^{3+}$ ions. The excitation spectra were composed of a broad band centered at 293 nm and weak multiline peaked in the range of 230~320 nm, which were due to the transitions of $Dy^{3+}$ ions. The emission of the phosphors peaking at 666 and 754 nm, originating from the transitions of $^4F_{9/2}{\rightarrow}^6H_{11/2}$ and $^4F_{9/2}{\rightarrow}^6H_{9/2}$ of $Dy^{3+}$ ions, was rather weak, while the intensity of blue and yellow emission peaking at 486 nm and 577 nm due to the transitions of $^4F_{9/2}{\rightarrow}^6H_{15/2}$ and $^4F_{9/2}{\rightarrow}^6H_{13/2}$ of $Dy^{3+}$ ions was significantly stronger. The experimental results suggest that the white-light emission can be realized by controlling the yellow-to-blue intensity ratio of $Dy^{3+}$ emission.