• Korean Journal of Chemical Engineering
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• 제36권2호
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• pp.191-196
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• 2019

The phase of Cu,Zn,Al precursors strongly affects the activity of their final catalysts. Herein, the Cu,Zn,Al precursor was prepared by precipitation of $Al^{3+}$ onto primitive, amorphous Cu,Zn precipitate. This precursor turned out to be a phase mixture of zincian malachite and hydrotalcite in which the latter phase was less abundant compared to the co-precipitated precursor. The final catalyst derived from this precursor exhibited a little higher copper surface area and methanol synthesis activity than the co-precipitated counterpart. Therefore, the two precursor phases need to be mixed in an adequate proportion for the preparation of active $Cu/ZnO/Al_2O_3$ catalyst.

• 한국세라믹학회지
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• 제35권5호
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• pp.458-464
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• 1998

Variations of reaction sequence of $Pb(Zn_{0.6}Mg_{0.4})_{1/3}Nb_{2/3}O_3$[PZMN] with precusor mixing methods were ex-amined using X-ray diffraction and dielectric characteristics. In the present study three different types of precursor mixing methods (oxide mixing PbO+$ZnNb_2O_6+MgNb_2O_6$[Zn+MN] and PbO+(Zn,Mg)$Nb_2O_6$[ZMN] precursor mixing) were adopted. When the oxide mixing method was used for the PZMN synthesis a Zn-rich perovskite phase and pyrochlore phase were formed. Compared with PbO+ZN+MN precursor mixing method the PbO-ZMN precursor led to a lowering of the formation temperature for perovskite sin-gle phase. These variation of composition and formation temperature of the perovskite phase were dis-cussed in terms of the difference in the solid-reaction requence between these three different types of pre-cursor mixing.

• 한국재료학회지
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• 제21권8호
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• pp.468-475
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• 2011

[ $LaMeO_3$ ](Me = Cr, Co) powders were prepared using the polymeric precursor method. The effects of the chelating agent and the polymeric additive on the synthesis of the $LaMeO_3$ perovskite were studied. The samples were synthesized using ethylene glycol (EG) as the solvent, acetyl acetone (AcAc) as the chelating agent, and polyvinylpyrrolidone (PVP) as the polymer additive. The thermal decomposition behavior of the precursor powder was characterized using a thermal analysis (TG-DTA). The crystallization and particle sizes of the $LaMeO_3$ powders were investigated via powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and particle size analyzer, respectively. The as-prepared precursor primarily has $LaMeO_3$ at the optimum condition, i.e. for a molar ratio of both metal-source (a : a) : EG (80a : 80a) : AcAc (8a) inclusive of 1 wt% PVP. When the as-prepared precursor was calcined at $700^{\circ}C$, only a single phase was observed to correspond with the orthorhombic structure of $LaCrO_3$ and the rhombohedral structure of $LaCoO_3$. A solid-electrolyte impedance-metric sensor device composed of $Li_{1.5}Al_{0.5}Ti_{1.5}(PO_4)_3$ as a transducer and $LaMeO_3$ as a receptor has been systematically investigated for the detection of NOx in the range of 20 to 250 ppm at $400^{\circ}C$. The sensor responses were able to divide the component between resistance and capacitance. The impedance-metric sensor for the NO showed higher sensitivity compared with $NO_2$. The responses of the impedance-metric sensor device showed dependence on each value of the NOx concentration.

• Bulletin of the Korean Chemical Society
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• 제18권6호
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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.

• 한국재료학회지
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• 제4권4호
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• pp.472-476
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• 1994

질산납으로부터 침전법으로 제조된 PbO-전구체의 상변태를 열분석, X-선 회절, 적외선 흡수 및 Raman분광 분석 등을 통하여 조사하였다. 질산납 수용액으로부터 $45^{\circ}C$, pH 9.0의 반응조건에서 PhO-전구체를 제조하였다. 침전물은 hydrous lead oxynitrate와 lead hydroxynitrate의 혼합체이었다. $560^{\circ}C$까지 열처리온도가 증가함에 따라 전구체는 $3Pb(NO_{3})_{2}$ㆍ7PbO를 거쳐 $Pb(NO_{3})_{2}$ㆍ5PbO로 된 후에 PbO(litharge)로 변화되었으며, $560^{\circ}C$이상에서 최종적으로 massicot형의 PbO로 변태되었다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2005년도 추계학술대회 논문집 Vol.18
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• pp.242-243
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• 2005

In this study, (La,Sr)$MnO_{3+\delta}$ powder used cathode material for SOFC was synthesized with precursor by GNP and the properties of powder, crystal phase, electric properties and deoxidization properties with precursor were investigated. The synthesis powder was prepared when oxidant/fuel mole and pH were 1 and 1, respectively and the synthesis powder was synthesized by GNP method using nitrate solution or oxide solution as precursor. Deoxidization peak of the nitrate solution was appeared lower temperature than the oxide solution, at $450^{\circ}C$. In this result, synthesis (La,Sr)$MnO_{3+\delta}$ powder using nitrate solution with Mn excess was suitable cathode material for SOFC due to had higher deoxidization properties. Also synthesis (La,Sr)$MnO_{3+\delta}$ powder according to precursor had difference electrical conductivity according to influence sintering density and crystal phase with precursor. Specially, the synthesis method and starting material had effect on deoxidization properties for SOFC.

• 한국세라믹학회지
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• 제33권8호
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• pp.915-920
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• 1996

콜로이드 졸-겔법에 의해 초미립자 mullite 분말을 제조하였다. Al2O3의 출발 물질로 aluminum isopropoxide $[Al(i-OC_3H_7)_3]$을, $SiO_2$ 출발 물질로 규산 나트륨으로부터 tetrahydrofuran(이후 THF로 약기함)으로 추출한 규산을 사용하였다. 규산 나트륨은 규산을 생성시키기 위하여 묽은 황산으로 산성화시킨 다음 THF로 추출하였다. Mullite 분말은 졸-겔법에 의해서 Si 추출율와 Na 제거율을 조사한 규산과 aluminum isopropoxide로 부터 합성되었다. THF로 추출한 규산의 불순물 함량은 0.04% 이하이었다. 합성된 mullite 분말은 $3Al_2O_3{\cdot}2SiO_2$ 조성을 갖고 불순물의 함량은 0.0462% 이하의 직경 $0.05{\mu}m$ 정도의 결정상이었다. EDS, XRD, TG/DSC, SEM, FT-IR, ICP, TEM등으로 mullite 분말의 특성을 조사하였다.

• 한국분말재료학회지
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• 제22권5호
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• pp.350-355
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• 2015

Perforated polygonal cobalt oxide ($Co_3O_4$) is synthesized using electrospinning and a hydrothermal method followed by the removal of a carbon nanofiber (CNF) template. To investigate their formation mechanism, thermogravimetric analysis, field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy are examined. To obtain the optimum condition of perforated polygonal $Co_3O_4$, we prepare three different weight ratios of the Co precursor and the CNF template: sample A (Co precursor:CNF template- 10:1), sample B (Co precursor:CNF template-3.2:1), and sample C (Co precursor:CNF template-2:1). Among them, sample A exhibits the perforated polygonal $Co_3O_4$ with a thin carbon layer (5.7-6.2 nm) owing to the removal of CNF template. However, sample B and sample C synthesized perforated round $Co_3O_4$ and destroyed $Co_3O_4$ powders, respectively, due to a decreased amount of Co precursor. The increased amount of the CNF template prevents the formation of polygonal $Co_3O_4$. For sample A, the optimized weight ratio of the Co precursor and CNF template may be related to the successful formation of perforated polygonal $Co_3O_4$. Thus, perforated polygonal $Co_3O_4$ can be applied to electrode materials of energy storage devices such as lithium ion batteries, supercapacitors, and fuel cells.

• 한국재료학회지
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• 제23권2호
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• pp.143-148
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• 2013

Well-distributed $SnO_2$-Sn-$Ag_3Sn$ nanoparticles embedded in carbon nanofibers were fabricated using a co-electrospinning method, which is set up with two coaxial capillaries. Their formation mechanisms were successfully demonstrated. The structural, morphological, and chemical compositional properties were investigated by field-emission scanning electron spectroscopy (FESEM), bright-field transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). In particular, to obtain well-distributed $SnO_2$ and Sn and $Ag_3Sn$ nanoparticles in carbon nanofibers, the relative molar ratios of the Ag precursor to the Sn precursor including 7 wt% polyacrylonitrile (PAN) were controlled at 0.1, 0.2, and 0.3. The FESEM, bright-field TEM, XRD, and XPS results show that the nanoparticles consisting of $SnO_2$-Sn-$Ag_3Sn$ phases were in the range of ~4 nm-6 nm for sample A, ~5 nm-15 nm for sample B, ~9 nm-22 nm for sample C. In particular, for sample A, the nanoparticles were uniformly grown in the carbon nanofibers. Furthermore, when the amount of the Ag precursor and the Sn precursor was increased, the inorganic nanofibers consisting of the $SnO_2$-Sn-$Ag_3Sn$ nanoparticles were formed due to the decreased amount of the carbon nanofibers. Thus, well-distributed nanoparticles embedded in the carbon nanofibers were successfully synthesized at the optimum molar ratio (0.1) of the Ag precursor to the Sn precursor after calcination of $800^{\circ}C$.

• 한국초전도ㆍ저온공학회논문지
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• 제7권3호
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• pp.5-8
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• 2005

Superconducting YBCO films were successfully fabricated by MOD process using F-free Cu precursor solution. In this study. a chemically modified precursor solution for MOD Processing was synthesized using metal-organic salts and F-free Cu precursor. It was shown that crack-free and uniform precursor films were formed after calcination in humidified oxygen atmosphere. Less than 3 hours are required to finish the calcination process. XRD measurement shows that $BaF_2,\;CuO,\;Y_2O_3$ are major constituent of precursor films. Furthermore. YBCO films without any secondary phases were successfully fabricated after annealing in wet $Ar/O_2$ prepared on a $LaA1O_3$ single crystal substrate $(10mm{\times}10mm)$ gives transport Ic of 10A at 77K. This chemical modification approach is a possible candidate for improving MOD-processing of YBCO coated conductor.