• Bulletin of the Korean Chemical Society
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• v.18 no.6
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• pp.612-618
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• 1997

$LiMn_2O_4$ powders were prepared by burning and subsequent calcination of PEG-metal nitrate precursor. After the burning stage of the precursor, some minor phases such as $Mn_2O_3$ (or $Mn_3O_4$), MnO, and carbonate were formed and single phases of $LiMn_2O_4$ were obtained by further calcinations above 400 ℃. From thermal analysis of the precursor, a violent thermal decomposition, which was indicated by a drastic weight loss accompanied by a sharp and strong exothermic peak, was observed and probably caused by an oxidation-reduction reaction between oxidizer and fuel. The formation of the minor phases could be explained in terms of the burning behavior of the precursor by employing valence concepts of propellant chemistry. The calcined powders were composed of submicron-sized but highly agglomerated particles and showed very broad particle size distribution.

• Electrical & Electronic Materials
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• v.10 no.2
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• pp.141-149
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• 1997

L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders were prepared by both GNP(Glycine-Nitrate Process) and solid state reaction method in various of calcination temperature(800-1000.deg. C) and time in air. Also, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contacts on YSZ(Yttria-Stabilized Zirconia) substrate were prepared by screen printing and sintering method as a function of sintering temperature(1100-1450.deg. C) in air. Sintering behaviors have been investigated by SEM(Scanning Electron Microscope) and porosity measurement. Compositional and structural characterization were carried out by X-ray diffractometer and ICP AES(Inductively Coupled Plasma-Atomic Emission Spectrometry) analysis. Electrical characterization was carried out by the electrical conductivity with linear 4 point probe method. As the calcination period increased in solid state reaction method, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ phase increased. Although L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ single phase was obtained only for 48hrs at 1000.deg. C, in GNP method it was easy to get single and ultra-fine L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders with submicron particle size at 650.deg. C for 30min. The particle size and thickness of L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contact by solid state reaction method did not change during the heat treatment, while those by GNP method showed good sintering characteristics because initial powder size fabricated from GNP method is smaller than that fabricated from solid state reaction method. Based on enthalpy change from thermodynamic data and ICP-AES analysis, it was suggested to make cathode contact in composition of (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$ Mn $O_{3}$ which have little second phase (L $a_{2}$Z $r_{2}$ $O_{7}$) for high efficient solid oxide fuel cells applications. As (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$Mn $O_{3}$ cathode contact on YSZ substrate was sintering at 1250.deg. C the temperature that liquid phase sintering did not occur. It was possible to obtain proper cathode contacts with electrical conductivity of 150(S/cm) and porosity content of 30-40%.m) and porosity content of 30-40%.

• The Korean Journal of Ceramics
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• v.4 no.3
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• pp.213-221
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• 1998

$BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder was synthesized by oxalate coprecipitation method. Precipitate with a stoichimetric ratio of the cations was prepared by adding a mixture of Ba, Ce and Gd nitrate solution to an oxalic acid solution at pH 4. Reaction between the constituent oxides to form a perovskite phase was initiated at $800^{\circ}C$ and a single phase $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder having good sinterability was obtained after calcination at $1000^{\circ}C$. Sintering green compacts of this powder for 6 h showed a considerable densification to start at $1100^{\circ}C$ and resulted in 93% and 97% relative densities at $1300^{\circ}$ and at $1450^{\circ}C$, respectively. Whereas the power compacts prepared by solid state reaction had lower relative densities, 78% at $1300^{\circ}$and 90% at $1450^{\circ}C$. Fine particles of $CeO_2$ second phase were observed in the surface of the sintered compacts. This was attributed to the evaporation of BaO from the surface that had been exposed during thermal etching.

• Journal of Powder Materials
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• v.19 no.4
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• pp.271-277
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• 2012

$SnO_2$ nanotubes were successfully synthesized using an electrospinning technique followed by calcination in air. The nanotubes were the single phase nature of $SnO_2$ and consisted of approximately 14 nm nanocrystals. SEM and TEM characterizations demonstrated that uniform hollow fibers with an average outer diameter of around 124 nm and wall thickness of around 25 nm were successfully obtained. As anode materials for lithium ion batteries, the $SnO_2$ nanotubes exhibited excellent cyclability and reversible capacity of $580mAhg^{-1}$ up to 25 cycles at $100mAg^{-1}$ as compared to $SnO_2$ nanoparticles with a capacity of ${\sim}200mAhg^{-1}$. Such excellent performance of the $SnO_2$ nanotube was related to the one-dimensional hollow structure which acted as a buffer zone during the volume contraction and expansion of Sn.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.14 no.11
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• pp.904-911
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• 2001

High-density lead zirconate titanate(Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$, PZT) ceramics were fabricated by a new milling-precipitation(MP) process improved from the conventional solid state process. This process was progressed by a milling impregnation through mixing ZrO$_2$ and TiO$_2$ powders with lead nitrate(Pb(NO$_3$)$_2$) water solution in zirconia ball media, and then milling precipitation was induced from precipitation of PbC$_2$O$_4$ by adding ammonium of oxalate monohydrate((NH$_4$)$_2$C$_2$O$_4$$.$H$_2$O) as a precipitant. As a result of this process, single-phase perovskite structure was formed at the calcination temperature of 750$\^{C}$ for Pb(Zr$\_$0.53/Ti$\_$0.47/)O$_3$ powders. In addition, the highest density at the sintering temperature of 1100$\^{C}$ was obtained, because of the highly sinterable PZT Powders ground through the re-milling process. Piezoelectric and dielectric properties of sintered sample were improved by MP process.

• Journal of the Korean Electrochemical Society
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• v.10 no.4
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• pp.288-294
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• 2007

The LSCF cathode far Solid Oxide Fuel Cell was investigated to develop high performance unit cell at intermediate temperature by modified oxalate method with different electrolytes and different pH. The LSCF powders employed La, Sr, Co and Fe oxides, oxalic acid, ethanol and $NH_4OH$ solution were synthesized with pH controlled as 2, 6, 7, 8, 9 and 10 at $80^{\circ}C$ Single crystalline phase was obtained from pH $2{\sim}9$. on the other hand, $La_2O_3$ appeared from pH 10. Very fine powder with particle size of 50 nm was obtained at calcination temperature of $800^{\circ}C$ for 4 hours. LSCF cathode synthesized at pH 7 showed the highest electric conductivity in the temperature range of $600^{\circ}C$ to $900^{\circ}C$ its value was 950 S/cm at $900^{\circ}C$ Under same synthesis conditions, polarization resistance of each LSCF cathode was changed with different calcination temperatures. As-prepared powder presented 2.52, 1.54 and $2.58\;{\Omega}$ at $600^{\circ}C$ with ScSZ, 8Y-YSZ and GDC as its electrolyte respectively after calcination at $800^{\circ}C$ for 4 hours.

• Journal of the Korean Magnetics Society
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• v.15 no.5
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• pp.282-286
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• 2005

Ni-Cu-Zn ferrites were prepared by the co-precipitation and ferrite microwave absorbers on low temperature sintering were investigated in this work. The properties of its microwave absorbing and physical were analyzed into variations of Ni addition, calcination temperature, sintering temperature. From the analysis of X-ray diffraction patterns, we can see that all the particles have only a single phase spinel structure. In addition, the powders particle size distribution obtained the nano size. By increasing the Ni additive, the permeability of the powders was decreased and the loss factor increased at sintering temperature $1100^{\circ}C$. Also, we considered that it can used high frequency rage. We found that the $(Ni_{0.7}Cu_{0.2}Zn_{0.1}O)_{1.02}(Fe_{2}O_3)_{0.98}$ appeared microwave absorbing properties better than other composition.

• Journal of the Korean Ceramic Society
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• v.51 no.5
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• pp.505-510
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• 2014

The properties of black ceramic pigments including thermal and glaze stability were systematically investigated so that these pigments could be used to decorate porcelain products. Various compositions of $(Ni,Mn)(Fe,Cr,Mn)_2O_4$ and $Co(Fe,Cr)_2O_4$ powders were synthesised using a solid state reaction method. The obtained $Co(Fe,Cr)_2O_4$ and $(Ni,Mn)(Fe,Cr,Mn)_2O_4$ powders showed single phases of spinel structure after calcination processes at $1000^{\circ}C$ and $1200^{\circ}C$, respectively. CIE $L^*a^*b^*$ colourimetric parameters of glazed $Co(Fe,Cr)_2O_4$ and $(Ni,Mn)(Fe,Cr,Mn)_2O_4$ pigments were analyzed according to the different amounts of Cr substitution. In addition, the amount of $Cr^{+6}$ remaining in the $Co(Fe,Cr)_2O_4$ and $(Ni,Mn)(Fe,Cr,Mn)_2O_4$ pigments was also measured.

• Advances in Energy Research
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• v.5 no.1
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• pp.13-29
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• 2017

The roles of Na, Mn, W and silica, and the synergistic effects between each metal in the $MnNa_2WO_4/SiO_2$ catalyst have been investigated for oxidative coupling of methane (OCM). The crystallisation of amorphous silica during calcination at $900^{\circ}C$ was promoted primarily by Na, but Mn and W also facilitated this process. The interaction between Na and Mn tended to increase the extent of conversion of $Mn_3O_4$ to $Mn_2O_3$. The formation of $Na_2WO_4$ was dependent on the order in which Na and W were introduced to the catalyst. The impregnation of W before Na resulted in the formation of $Na_2WO_4$, but this did not occur when the impregnation order was reversed. $MnWO_4$ formed in all cases where Mn and W were introduced into the silica support, regardless of the impregnation order; however, the formation of $MnWO_4$ was inhibited in the presence of Na. Of the prepared samples in which a single metal oxide was introduced to silica, only $Mn/SiO_2$ showed OCM activity with significant oxygen conversion, thus demonstrating the important role that Mn plays in promoting oxygen transfer in the reaction. The impregnation order of W and Na is critical for catalyst performance. The active site, which involves a combination of Na-Si-W-O, can be formed in situ when distorted $WO_4^{2-}$ interacts with silica during the crystallisation process facilitated by Na. This can only occur if the impregnation of W occurs before Na addition, or if the two components are introduced simultaneously.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.4
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• pp.195-200
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• 2013

Novel Sr-Y-Si-Oxynitride yellow phosphors were synthesized and the effect of calcination temperature, reduction temperature and $Eu^{2+}$ concentration on their luminescence properties were studied. Optimal temperature conditions were found to be $1400^{\circ}C$ and $1300^{\circ}C$ for solid-state reaction and reduction, respectively. The synthesized $Ba_9Y_{2+y}Si_6O_{24-3y}N_{3y}:Eu^{2+}$ phosphors showed a single intense broadband emission in the range of 571~587 nm for 450 nm excitation light source. The highest luminescence intensity was obtained with Eu concentration of 3 mol% and concentration quenching was observed beyond 5 mol%. FE-SEM and PSA showed that the synthesized phosphors consists of particles with an average size of ${\sim}8.2{\mu}m$.