• Title/Summary/Keyword: Precursor Powder

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Synthesis and Characterization of CNT / TiO2 Photoelectrocatalytic Electrodes for Methlene Blue Degradation

  • Zhang, Feng-Jun;Chen, Ming-Liang;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.18 no.11
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    • pp.583-591
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    • 2008
  • In this study, two series of CNT/$TiO_2$ electrodes were prepared. The decrease of surface area compared with that of the pristine carbon nanotubes (CNTs) indicated the blocking of micropores on the surface of the CNTs; was further supported by scanning electron microscopy (SEM) and field emission SEM (FE-SEM) observations. The X-ray diffraction (XRD) results showed that the CNT/$TiO_2$ composites contained a mix of anatase and rutile forms of $TiO_2$ particles when the precursor was $TiO_2$ powder, whereas when the precursor was Ti ($OC_4H_7$) (TNB), the composites contained only the typical single and clear anatase $TiO_2$ particles. The energy dispersive X-ray spectroscopy (EDX) spectra showed the presence of C, O and Ti peaks for all samples. It was found that catalytic decomposition of methylene blue (MB) solution could be attributed to synthetic effects between the $TiO_2$ photocatalysis and electro-assisted CNTs network, and that photoelectrocatalytic oxidation increased with an increase of CNT composition. It was also found that the photoelectrocatalytic oxidation efficiency for MB is higher than that of photocatalytic oxidation. Moreover, the CNT/$TiO_2$ composites catalyst prepared by the impregnation method demonstrates higher photoelectrocatalytic activity than the mechanical mixture with the same CNT content.

Fabrication of Spherical SiO2 Powders from Aqueous SiO2 Sol via Ultrasonic Pyrolysis (초음파 분무 열분해 공정을 이용한 수계 SiO2 Sol로부터의 구형 SiO2 분말 합성)

  • Lee, Ji-Hyeon;Hwang, Hae-Jin;Han, Kyu-Sung;Hwang, Kwang-Taek;Kim, Jin-Ho
    • Korean Journal of Materials Research
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    • v.26 no.10
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    • pp.570-576
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    • 2016
  • Using the ultrasonic pyrolysis method, spherical $SiO_2$ powders were synthesized from aqueous $SiO_2$ sol as a starting material. The effects of pyrolysis conditions such as reaction temperature, $SiO_2$ sol concentration, and physical properties of precursor were investigated for the morphologies of the resulting $SiO_2$ powders. The particle size, shape, and crystallite size of the synthesized $SiO_2$ powders were demonstrated according to the pyrolysis conditions. Generally, the synthesized $SiO_2$ particles were amorphous phase and showed spherical morphology with a smooth surface. It was revealed that increased crystallite size and decreased spherical $SiO_2$ particle size were obtained with increases of the pyrolysis reaction temperature. Also, quantity of spherical $SiO_2$ particles decreased with the decrease in the concentration and surface tension of the precursor.

Low Temperature Synthesis of BaCeO3 Nano Powders by the Citrate Process (Citrate Process를 이용한 BaCeO3 나노 분말의 저온 합성)

  • Lee, Dong-Wook;Won, Jong-Han;Joo, Kyoung;Kim, Chang-Yeoul;Shim, Kwang-Bo
    • Journal of the Korean Ceramic Society
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    • v.39 no.6
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    • pp.604-609
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    • 2002
  • Nanosized $BaCeO_3$ powders with the stoichiometric composition of a molecular level were synthesized by the citrate process based on the Pechini method. Polymeric precursor was formed by use of citric acid and ethylen glycol, as chelating agent of metal ions and reaction medium, respectively. Single phase orthorhombic structured $BaCeO_3$powders, about 100 nm sized and uniform shaped were obtained through the calcination of the polymeric precursor at $900^{\circ}C$ for 4 h. Extremely small quantities of carbonate ions($CO_^{2-}$) were completely decomposed at over $1100^{\circ}C$. The mean size of the powders was increased twice, however, it has very uniform distribution in its size and shape.

Synthesis of Silicon-Carbon by Polyaniline Coating and Electrochemical Properties of the Si-C|Li Cell

  • Doh, Chil-Hoon;Kim, Seong Il;Jeong, Ki-Young;Jin, Bong-Soo;An, Kay Hyeok;Min, Byung Chul;Moon, Seong-In;Yun, Mun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.27 no.8
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    • pp.1175-1180
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    • 2006
  • Si-C composites were prepared by the carbonization of polyaniline (PAn) coated on silicone powder. The physical and electrochemical properties of the Si-C composites were characterized by particle-size analysis, X-ray diffraction, scanning electron microscopy, and battery electrochemical tests. The average particle size of Si was increased by the coating of Pan but somewhat reduced by the carbonization to give silicone-carbon composites. The co-existence of crystalline silicone and amorphous-like carbon was confirmed by XRD analyses. SEM photos showed that the silicone particles were well covered with carbonaceous materials, depending on the PAn content. Si-C$\mid$Li cells were fabricated using the Si-C composites and tested using galvanostatic charge-discharge. Si-C$\mid$Li cells gave better electrochemical properties than Si|Li cells. Si-C$\mid$Li cells using Si-C from HCl-undoped precursor PAn showed better electrochemical properties than precursor PAn doped in HCl. The addition of an electrolyte containing 4-fluoroethylene carbonate (FEC) increased the initial discharge capacity. Also, another electrochemical test, the galvanostatic charge-discharge test with GISOC (gradual increasing of the state of charge) was carried out. Si-C(Si:PAn = 50:50 wt. ratio)|Li cell showed 414 mAh/g of reversible specific capacity, 75.7% of IIE (initial intercalation efficiency), 35.4 mAh/g of IICs (surface irreversible specific capacity).

Conformations and Vibrational Frequencies of a Precursor of Benzovesamicol Analogues Studied by Density Functional Theories

  • Park, Jong-Kil;Choe, Sang Joon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2311-2316
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    • 2014
  • Conformations and vibrational frequencies of the racemic (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalen-2-ol-(I) [(2RS,3RS)-(I)], a precursor of benzovesamicol analogues, have been carried out using various DFT methods (M06-2X, B3LYP, B3PW91, PBEPBE, LSDA, and B3P86) with basis sets of 6-31G(d), 6-31+G(d,p), 6-311+G(d,p), 6-311++G(d,p), cc-pVTZ, and TZVP. The LSDA/6-31G(d) level of theory shows the best performance in reproducing the X-ray powder structure. However, the PBEPBE/cc-pVTZ level of theory is the best method to predict the vibrational frequencies of (2RS,3RS)-(I). The potential energy surfaces of racemic pairs (2RS,3RS)-(I) and -(II) are obtained at the LSDA/6-31G(d) level of theory in the gas phase and in water. The results indicate that (2RS,3RS)-(I) are more stable by ~0.75 kcal/mol in energy than (2RS,3RS)-(II) in water, whereas conformer AIIg and BIIg are more stable by ~0.04 kcal/mol than AIg in gas phase. In particular, the hydrogen bond distances between the N of piperazine and the OH of tetrahydronaphthalen become longer in gas, compared with those in the water phase. Vibrational frequencies calculated at the PBEPBE/cc-pVTZ level of theory in the gas phase are larger than those in water, whereas their intensities in the gas phase are weaker than those in water.

Fabricatiion and Characterization of ${Bi_2}{Sr_2}{CaCu_2}{O_8}$ Superconductor Thick Films on Cu Substrates using Cu-free Precursors (Cu-free 전구체를 이용하여 구리 기판 위에 ${Bi_2}{Sr_2}{CaCu_2}{O_8}$ 초전도 후막의 제조 및 특성)

  • 한상철;김상준;한영희;성태현;한병성
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.13 no.4
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    • pp.349-358
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    • 2000
  • Fabrication and Characterization of Bi$_{2}$/Sr$_{2}$/CaCu$_{2}$/O$_{8}$(Bi2212) superconductor thick films were fabricated successfully on C tapes by liquid reaction between Cu-free precursors of Bi$_{x}$/SrCaO/$_{y}$(x=1.2-2) and Cu tapes. Cu-free Bi-Sr-Ca-O powder mixtures were screen-printed on Cu tapes and heat-treated at 850-87$0^{\circ}C$ for several minutes in air oxygen nitrogen and low oxygen pressure. In order to obtain the optimum heat-treatment condition we studied the effect of the precursor composition the printing thickness and the heat-treatment atmosphere on the superconducting properties of Bi2212 films and the reaction mechanism. Microstructures and phases of thick films were analyzed by films and the reaction mechanism. Microstructures and phases of thick films were analyzed by optical microscope and XRD. The electric properties of superonducting films were examined by the four probe method. At heat-treatment temperature the thick films were in a partially molten state by liquid reaction between CuO of the oxidized copper tape and the precursors which were printed on Cu tapes. During the heat-treatment procedure Bi2212 superconducting particle nucleate and grow in preferred orientations.ons.s.

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Effect of Sulfurization Temperature on the Properties of Cu2ZnSn(S,Se)4 Thin Films (황화 열처리 온도에 따른 Cu2ZnSn(S,Se)4 박막의 합성 및 특성 평가)

  • Yoo, Yeong Yung;Hong, Chang Woo;Gang, Myeng Gil;Shin, Seung Wook;Kim, Young Baek;Moon, Jong-Ha;Lee, Yong Jeong;Kim, Jin Hyoek
    • Korean Journal of Materials Research
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    • v.23 no.11
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    • pp.613-619
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    • 2013
  • $Cu_2ZnSn(S_x,Se_{1-x})_4$ (CZTSSe) thin films were prepared by sulfurization of evaporated precursor thin films. Precursor was prepared using evaporation method at room temperature. The sulfurization was carried out in a graphite box with S powder at different temperatures. The temperatures were varied in a four step process from $520^{\circ}C$ to $580^{\circ}C$. The effects of the sulfurization temperature on the micro-structural, morphological, and compositional properties of the CZTSSe thin films were investigated using X-ray diffraction (XRD), Raman spectra, field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The XRD and Raman results showed that the sulfurized thin films had a single kesterite crystal CZTSSe. From the FE-SEM and TEM results, the $Mo(S_x,Se_{1-x})_2$ (MoSSe) interfacial layers of the sulfurized CZTS thin films were observed and their thickness was seen to increase with increasing sulfurization temperature. The microstructures of the CZTSSe thin films were strongly related to the sulfurization temperatures. The voids in the CZTSSe thin films increased with the increasing sulfurization temperature.

Fabrication of Y2O3 doped ZrO2 Nanopowder by Reverse Micelle and Sol-Gel Processing

  • Kim, Hyun-Ju;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.21 no.10
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    • pp.568-572
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    • 2011
  • The preparation of $Y_2O_3$-doped $ZrO_2$ nanoparticles in Igepal CO-520/cyclohexane reverse micelle solutions is studied here. In this work, we synthesized nanosized $Y_2O_3$-doped $ZrO_2$ powders in a reverse micelle process using aqueous ammonia as the precipitant. In this way, a hydroxide precursor was obtained from nitrate solutions dispersed in the nanosized aqueous domains of a microemulsion consisting of cyclohexane as the oil phase, with poly (oxyethylene) nonylphenylether (Igepal CO-520) as the non-ionic surfactant. The synthesized and calcined powders were characterized by thermogravimetrydifferential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The crystallite size was found to nearly identical with an increase in the water-to-surfactant (R) molar ratio. A FTIR analysis was carried to monitor the elimination of residual oil and surfactant phases from the microemulsion-derived precursor and the calcined powder. The average particle size and distribution of the synthesized $Y_2O_3$-doped $ZrO_2$ were below 5 nm and narrow, respectively. The TG-DTA analysis showed that the phase of the $Y_2O_3$-doped $ZrO_2$ nanoparticles changes from the monoclinic phase to the tetragonal phase at temperatures close to $530^{\circ}C$. The phase of the synthesized $Y_2O_3$-doped $ZrO_2$ when heated to $600^{\circ}C$ was tetragonal $ZrO_2$.

Properties of Synthesis (BaSr)$(CoFe)O_3$ Cathode for IT-SOFC by GNP (GNP 법을 이용한 저온형 SOFC용 (BaSr)$(CoFe)O_3$ 공기극의 제조 및 특성 평가)

  • Lee, Mi-Jai;Moon, Ji-Woong;Kim, Sei-Ki;Ji, Mi-Jung;Hwang, Hae-Jin;Lim, Yong-Ho;Choi, Byung-Hyun
    • 한국신재생에너지학회:학술대회논문집
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    • 2006.06a
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    • pp.51-54
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    • 2006
  • Cathode material, $(Ba_{0.5}Sr_{0.5})_{0.99}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$, for low temperature SOFC was prepared by the glycine-nitrate synthesis process (GNP). The characteristics of the synthesized powders were studied with controlling pH of a precursor. The synthesis BSCF powders with pH were agglomeration state and calcinations temperature has not influence on particles. Highly acidicprecursor solution increased a single phase forming the temperature. Also, synthesis BSCF powder was show result for thermal analysis and alteration of difference crystal with pH. It is considered that Ba and Sr cannot complex by carboxylic acid group of glycine, because under highly acidic condition the caboxylic group mainly combined with $H^+$ insead of alkali and alkaline earth cations. In case of using precursor solution with pH $2{\sim}3$, a single perovskite phase was obtained at $1000^{\circ}C$. Polarization resistance of $(Ba_{0.5}Sr_{0.5})_{0.99}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ was measured by AC impedance spectroscopy from the two electrode symmetric cell. Area specific resistance of the $(Ba_{0.5}Sr_{0.5})_{0.99}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ air electrode at $500^{\circ}C\;and\;600^{\circ}C$ were $0.96{\Omega}?cm^2$ and $0.16{\Omega}?cm^2$, respectively.

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Oxygen Permeation Properties of La0.7Sr0.3Co0.3Fe0.7O3-δ Membrane (La0.7Sr0.3Co0.3Fe0.7O3-δ 분리막의 산소투과특성)

  • Son, Sou Hwan;Kim, Jong-Pyo;Park, Jung Hoon;Lee, Yongtaek
    • Korean Chemical Engineering Research
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    • v.47 no.3
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    • pp.310-315
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    • 2009
  • Perovskite-type ceramic powder, $La_{0.7}Sr_{0.3}Co_{0.3}Fe_{0.7}O_{3-{\delta}}$, have been synthesized successfully by the citrate method. As a result of TGA for precursor, metal-citrate complex in precursor was decomposed in the temperature range of $150{\sim}650^{\circ}C$. XRD analysis showed the single perovskite structure was observed over $1,000^{\circ}C$ without impurities. Typical dense membrane with 1.6 mm thickness has been prepared using as-prepared powder by pressing unilaterally and sintering at $1,300^{\circ}C$. The electrical conductivity of $La_{0.7}Sr_{0.3}Co_{0.3}Fe_{0.7}O_{3-{\delta}}$ membrane increased with increasing temperature at atmosphere of air and then decreased over $600^{\circ}C$ due to oxygen loss from the crystal lattice. The oxygen flux of $La_{0.7}Sr_{0.3}Co_{0.3}Fe_{0.7}O_{3-{\delta}}$ membrane in the range of 700 to $950^{\circ}C$ increased with the increasing temperature from 0.045 to $0.415ml/cm^2{\cdot}min$. The activation energy for oxygen permeation was calculated to be 89.17 kJ/mol.