• Title/Summary/Keyword: Solid state synthesis

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Synthesis and Formation Mechanism of ZrTiO4 Gray Pigment (ZrTiO4계 Gray 안료 합성과 형성기구)

  • Hwang, Dong-Ha;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.84-89
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    • 2012
  • Attempts were made to develop a stable gray pigment at reducing atmosphere, substituting Ti in $ZrTiO_4$ with Mn, Fe, Co and Cu The pigment synthesized at $1300~1500^{\circ}C$ by solid state method with the composition of $ZrTi_{1-x-y}A_xB_yO_4$ (x = y = 0.005, 0.015, 0.035, 0.055, 0.075, 0.095, 0.115, 0.135, 0.155, 0.175 and 0.195 mole, A = Mn(III), Fe(III), Co(II, III) and Cu(II) (chromophores), B = Sb (counterion). The pigments were fired at $1400^{\circ}C$ for 3 h with substitute amount changes of Mn, Fe, Co and Cu to $ZrTiO_4$ crystals, and analyzed by Raman spectroscopy to figure out substitute limits. Results indicated 0.035 mole for Mn, 0.115 mole for Fe, 0.015 mole for Co and 0.015 mole for Cu as substitute limits, respectively. Figs. 1, 2, 3, and 4 represent each substitute pigments of Mn, Fe, Co and Cu. Synthesized pigment was applied to a lime and a lime-magnesia glaze at 7 wt% each, and fired at reducing atmosphere of $1240^{\circ}C$, soaking time 1h. Gray color was obtained with CIE-$L^*a^*b^*$ values at 44.55, -0.65, 1.19(Mn), 40.36, -0.90, 0.30(Fe), 42.63, -0.03, -1.49(Cu) and -40.79, -0.28, -0.91(Co), respectively.

Synthesis and Characterization of Phenylene-Thiophene-Thieno[3,4-b]pyrazine Oligomer (Phenylene-Thiophene-Thieno[3,4-b]pyrazine 올리고머의 합성과 특성)

  • Hwang, Mi-Lim;Li, Ji-Cheng;Seo, Eun-Ok;Lee, Soo-Hyoung;Lee, Youn-Sik
    • Korean Chemical Engineering Research
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    • v.49 no.1
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    • pp.95-100
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    • 2011
  • During the development of low band-gap organic materials(p-type semiconducting organic compounds) for organic solar cells, an oligomer consisting of 2,5-dioctyloxyphenylene(OP), 3-hexylthiophene(HT), and 2,3-dimethylthieno[ 3,4-b]pyrazine(TP) as repeat units, oligo(OP-HT-TP), was synthesized. The oligomer was amorphous in nature in the temperature range studied, and well soluble in common organic solvents such as chloroform. The maximum absorption wavelength was 716 nm in solid state. The band-gap and HOMO/LUMO energy levels of oligo(OP-HT-TP) were measured to be 1.20 eV and -5.27/4.04 eV, respectively. However, the absorbance of the oligomer at maximum absorption wavelength was less than one fifth of that of poly(3-hexylthiophene) which has been most frequently used in fabrication of organic solar cells.

Synthesis of Nano Size $BaCeO_3$ as an Effective Flux Pining Center for YBCO Superconductor (YBCO 초전도체의 효과적인 플럭스 피닝 센터로서의 나노 크기 $BaCeO_3$ 합성)

  • Youn, J.S.;No, K.S.;Kim, Y.H.;Jun, B.H.;Lee, J.P.;Jung, S.Y.;Kim, C.J.
    • Progress in Superconductivity
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    • v.10 no.1
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    • pp.12-16
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    • 2008
  • In this work, nano size $BaCeO_3$, which is a possible flux pinning medium of melt processed $YBa_{2}Cu_{3}O_x$ superconductor, was synthesized by the conventional solid state reaction method using powders. $BaCeO_3$ and $CeO_2$ were mixed thoroughly using a ball milling for 24 hours and calcined at $1200^{\circ}C$ for 5 hours for the formation $BaCeO_3$ powder. The obtained $BaCeO_3$ powder was attrition milled at various milling times of 60 min, 120 min and 240 min. The $BaCeO_3$ powders of various milling times were mixed with $YBa_{2}Cu_{3}O_x$ powder. Seed melt processed $YBa_{2}Cu_{3}O_x$-$BaCeO_3$ (15wt.%) superconductors were prepared and the superconducting properties were investigated. It was found that $T_c$ of $Y_{1.5}Ba_{2}Cu_{3}O_x$ samples was not significantly affected by $BaCeO_3$ addition, but $J_c$ of samples was increased by $BaCeO_3$ addition. The $J_c$ improvement by fine $BaCeO_3$ powder (120 min attrition-milled) was effective at low magnetic fields less than 2 T.

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Thermal Development from Hybrid Gels of Compounds for Use in Fibre-Reinforced Oxide Ceramics

  • MacKenzie, Kenneth J.D.;Kemmitt, Tim;Meinhold, Richard H.;Schmucker, Martin;Mayer, Lutz
    • The Korean Journal of Ceramics
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    • v.4 no.4
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    • pp.323-330
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    • 1998
  • Mixed oxide compounds of potential usefulness for fibre coatings (hexagonal celsian, $BaAl_2Si_2O_8$ and lanthanum hexaluminate, $LaAl_{11}O_{18}$) or for matrix materials (yttrium aluminium garnet, $Y_3Al_5O_{12}$) were prepared by hybrid sol-gel synthesis and their thermal crystallisation was monitored by thermal analysis, X-ray diffraction and multinuclear solid state MAS NMR. All the gels convert to the crystalline phase below about $12200^{\circ}C$, via amorphous intermediates in which the Al shows and NMR resonance at 36-38 ppm sometimes ascribed to Al in 5-fold coordination. Additional information about the structural changes during thermal treatment was provided by $^{29}Si$, $^{137}Ba$ and $^{89}Y$ MAS NMR spectroscopy, showing that the feldspar framework of celsian begins to be established by about $500^{\circ}C$ but the Ba is still moving into its polyhedral lattice sites about $400^{\circ}C$ after the sluggish onset of crystallization. Lanthanum hexaluminate and YAG crystallise sharply at 1230 and $930^{\circ}C$ respectively, the former via $\gamma-Al_2O_3$, the latter via $YAlO_3$. Yttrium moves into the garnet lattice sites less than $100^{\circ}C$ after crystallisation.

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Synthesis and electrochemical properties of layered $Li[Ni_xCo_{1-2x}Mn_x]O_2$ materials for lithium secondary batteries prepared by mechanical alloying (기계적 합금법을 이용한 리튬 2차 전지용 층상 양극물질 $Li[Ni_xCo_{1-2x}Mn_x]O_2$ 의 합성 및 전기화학적 특성에 관한 연구)

  • 박상호;신선식;선양국
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.16-16
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    • 2002
  • The presently commercialized lithium-ion batteries use layer structured LiCoO₂ cathodes. Because of the high cost and toxicity of cobalt, an intensive search for new cathode materials has been underway in recent years. Recently, a concept of a one-to-one solid state mixture of LiNO₂ and LiMnO₂, i.e., Li[Ni/sub 0.5/Mn/sub 0.5/]O₂, was adopted by Ohzuku and Makimura to overcome the disadvantage of LiNiO₂ and LiMnO₂. Li[Ni/sub 0.5/Mn/sub 0.5/]O₂ has the -NaFeO₂ structure, which is characteristic of the layered LiCoO₂ and LiNiO₂ structures and shows excellent cycleability with no indication of spinel formation during electrochemical cycling. Layered Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂ (x = 0.5 and 0.475) materials with high homogeneity and crystallinity were synthesized using a mechanical alloying method. The Li[Ni/sub 0.475/Co/sub 0.05/Mn/sub 0.475/]O₂ electrode delivers a high discharge capacity of 187 mAh/g between 2.8 and 4.6 V at a high current density of 0.3 mA/㎠(30 mA/g) with excellent cycleability. The charge/discharge and differential capacity vs. voltage studies of the Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂ (x = 0.5 and 0.475) materials showed only one redox peak up to 50 cycles, which indicates that structural phase transitions are not occurred during electrochemical cycling. The magnitude of the diffusion coefficients of lithium ions for Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂(x = 0.5 and 0.475) are around 10/sup -9/ ㎠/s measured by the galvanostatic intermittent titration technique (GITT).

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Synthesis and luminescent properties of $Er^{3+}$ doped $CaZrO_3$ long persistent phosphors ($Er^{3+}$를 첨가한 $CaZrO_3$ 축광성 형광체의 합성 및 발광 특성 분석)

  • Park, Byeong-Seok;Choi, Jong-Koen
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.1
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    • pp.27-32
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    • 2008
  • Novel long persistent phosphors of $CaZrO_3:Er^{3+}$ have been synthesized by traditional solid state reaction method. The long persistent phosphor crystalline particles were characterized by the X-ray diffraction (XRD), photoluminescence spectrophotometer, thermoluminescence (TL) and luminance meter. The results reveal that the samples are composed of single $CaZrO_3$ phase. The broadband emission spectra of 446 nm peak and 550 nm peak was revealed by synthesized at high temperature in $N_2$ gas. Green long persistent phosphors have been observed in the sys_em for over 6 h after UV irradiation (254 nm). The main emission peak was ascribed to $Er^{3+}$ ions transition from $^5D_{5/2}{\rightarrow}^4F_{9/2},\;^2H_{12/2},\;^4S_{3/2}{\rightarrow}^4I_{13/2}\;and\;^2G_{9/2}{\rightarrow}^4I_{13/2}$, and the afterglow may be ascribed to the suitable trap centers in the $CaZrO_3$ host lattice.

Synthesis of SrGa2S4 Phosphor and Its Luminescent Properties (SrGa2S4 형광체의 합성과 발광 특성)

  • Heo, Yeong-Deok;Sim, Jae-Hun;Do, Yeong-Rak
    • Journal of the Korean Chemical Society
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    • v.46 no.2
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    • pp.164-168
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    • 2002
  • SrGa$_2$S$_4$ : Eu is a green emitting phosphor which is applied for field emission display, and cathodoluminescence. Conventionally, SrGa$_2$S$_4$ : Eu is synthesized by solid state reaction, in which a mixture of SrCO$_3$, Ga$_2$O$_3$, and Eu$_2$O$_3$ is fired at high temperatures under flowing H$_2$S and Ar gases. In this study,SrGa$_2$S$_4$ : Eu phosphor is synthesized by using a decomposition method, where SrS, Eu complex, and Ga com-plex are used. The advantage of this method is that toxic H$_2$S gas and Ar gas are not used. The synthetic con-ditions and luminescent properties of SrGa$_2$S$_4$ : Eu phosphor are also investigated.

Synthetic Characteristics of AlPO$_4$-5 Molecular Sieve (AlPO$_4$-5 분자체의 합성 특성)

  • Sung Hwa Jhung;Suk Bong Hong;Young Sun Uh;Hakze Chon
    • Journal of the Korean Chemical Society
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    • v.37 no.10
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    • pp.867-873
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    • 1993
  • Influences of crystallization time and $H_2O/Al_2O_3$ ratio of the reaction mixtures on the synthesis of AlPO$_4$-5 molecular sieve have been studied by X-ray powder diffraction, nitrogen adsorption, scanning electron microscope (SEM), and solid state $^{27}$Al magic angle spinning nuclear magnetic resonance (MAS NMR) techniques. The degree of crystallinity of AlPO$_4$-5 follows a sigmoid pattem as crystallization time increases. The induction period is shorter than 1 h when the crystallization process is carried out at 150$^{\circ}$C. The conversion of reactants to product, AlPO$_4$-5, can be clearly observed, and all of the determined physical properties change abruptly after about 2 h. It is found that increase in $H_2O/Al_2O_3$ ratio of the reaction mixtures not only changes the crystal morphology from aggregates to hexagonal single crystals, but also results in the formation of longer AlPO$_4$-5 crystals.

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Synthesis of Nanocrystalline ZnFe2O4 by Polymerized Complex Method for its Visible Light Photocatalytic Application: An Efficient Photo-oxidant

  • Jang, Jum-Suk;Borse, Pramod H.;Lee, Jae-Sung;Jung, Ok-Sang;Cho, Chae-Ryong;Jeong, Euh-Duck;Ha, Myoung-Gyu;Won, Mi-Sook;Kim, Hyun-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.30 no.8
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    • pp.1738-1742
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    • 2009
  • Nanocrystalline Zn$Fe_2O_4$ oxide-semiconductor with spinel structure was synthesized by the polymerized complex (PC) method and investigated for its photocatalytic and photoelectric properties. The observation of a highly pure phase and a lower crystallization temperature in Zn$Fe_2O_4$ made by PC method is in total contrast to that was observed in Zn$Fe_2O_4$ prepared by the conventional solid-state reaction (SSR) method. The band gap of the nanocrystalline Zn$Fe_2O_4$ determined by UV-DRS was 1.90 eV (653 nm). The photocatalytic activity of Zn$Fe_2O_4$ prepared by PC method as investigated by the photo-decomposition of isopropyl alcohol (IPA) under visible light (${\geq}$ 420 nm) was much higher than that of the Zn$Fe_2O_4$ prepared by SSR as well as Ti$O_{2-x}N_x$. High photocatalytic activity of Zn$Fe_2O_4$ prepared by PC method was mainly due to its surface area, crystallinity and the dispersity of platinum metal over Zn$Fe_2O_4$.

Synthesis and luminescence properties of $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ phosphors ($Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ 형광체의 합성과 발광 특성)

  • Sung, Hye-Jin;Huh, Young-Duk
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.16 no.6
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    • pp.267-272
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    • 2006
  • A series of $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ phosphors have been synthesized by solid-state reaction. The photoluminescence and structural properties of $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ have been examined. The $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ phosphors have a strong absorption at 400 nm, which is the emission wavelength of a violet light emitting diode (LED). The emission peaks of $SrGa_2S_4:Ce,Na$are located at 448 nm and 485 nm. The partial replacement of Sr by Ca in $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ causes a red shift of emission wavelengths. The $Sr_{1-x}Ca_xGa_2S_4:Ce,Na$ can be used as blue emitting phosphors pumped by the violet LED for fabricating the multi-band white LED.