• Title/Summary/Keyword: precursor method.

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Selective Oxidation of Hydrogen Over Palladium Catalysts in the Presence of Carbon Monoxide: Effect of Supports (Pd 촉매상에서 일산화탄소 존재 하 수소의 선택적 산화반응: 담체 효과)

  • Kim, Eun-Jeong;Kang, Dong-Chang;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.55 no.1
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    • pp.121-129
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    • 2017
  • Pd based catalysts were prepared by impregnating palladium precursor using incipient wetness method on $TiO_2$, $Al_2O_3$, $ZrO_2$, and $SiO_2$ and were applied for the selective oxidation of $H_2$ in the presence of CO. Their physicochemical properties were studied by X-ray diffraction (XRD), $N_2$-sorption, temperature programmed desorption of CO (CO-TPD) and (CO+$H_2O$)-TPD, temperature programmed reduction of CO (CO-TPR) and XPS a. The results of CO- and (CO+$H_2O$)-TPD showed the correlation between peak temperature of TPD and catalytic activities for $H_2$ and CO conversion. The $Pd/ZrO_2$ catalyst exhibited the highest conversion of $H_2$. The addition of $H_2O$ vapor promotes the conversion of $H_2$ and CO by inducing easy desorption of CO and $H_2$ in the competitive adsorption of $H_2O$, CO and $H_2$.

Electrochemical Properties of Spinel LiMn2O4 Prepared Through Different Synthesis Routes (스피넬형 양극활물질 LiMn2O4의 합성방법에 따른 전기화학적 특성 비교)

  • Lee, Ki-Soo;Bang, Hyun-Joo;Sun, Yang-Kook
    • Journal of the Korean Electrochemical Society
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    • v.10 no.1
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    • pp.48-51
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    • 2007
  • In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.

Preparation of LiFe PO4 Using Chitosan and its Cathodic Properties for Rechargeable Li-ion Batteries

  • Hong, Kyong-Soo;Yu, Seong-Mi;Ha, Myoung-Gyu;Ahn, Chang-Won;Hong, Tae-Eun;Jin, Jong-Sung;Kim, Hyun-Gyu;Jeong, Euh-Duck;Kim, Yang-Soo;Kim, Hae-Jin;Doh, Chil-Hoon;Yang, Ho-Soon;Jung, Hee
    • Bulletin of the Korean Chemical Society
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    • v.30 no.8
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    • pp.1719-1723
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    • 2009
  • The LiFeP$O_4$ powder was synthesized by using the solid state reaction method with Fe($C_2O_4){\cdot}2H_2O,\;(NH_4)_2HPO_4,\;Li_2CO_3$, and chitosan as a carbon precursor material for a cathode of a lithium-ion battery. The chitosan added LiFePO4 powder was calcined at 350 ${^{\circ}C}$ for 5 hours and then 800 ${^{\circ}C}$ for 12 hours for the calcination. Then we calcined again at 800 ${^{\circ}C}$ for 12 hours. We characterized the synthesized compounds via the crystallinity, the valence states of iron ions, and their shapes using TGA, XRD, SEM, TEM, and XPS. We found that the synthesized powders were carbon-coated using TEM images and the iron ion is substituted from 3+ to 2+ through XPS measurements. We observed voltage characteristics and initial charge-discharge characteristics according to the C rate in LiFeP$O_4$ batteries. The obtained initial specific capacity of the chitosan added LiFeP$O_4$ powder is 110 mAh/g, which is much larger than that of LiFeP$O_4$ only powder.

The Effect of Calcination Temperature on the Layered Li1.05Ni0.9Co0.05Ti0.05O2 for Lithium-ion Battery (리튬이온전지용 층상 Li1.05Ni0.9Co0.05Ti0.05O2에 대한 소성 온도의 영향)

  • Ko, Hyoung Shin;Park, Hyun Woo;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.56 no.5
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    • pp.718-724
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    • 2018
  • In this study, the $Ni_{0.9}Co_{0.05}Ti_{0.05}(OH)_2$ precursor was prepared by the concentration gradient co-precipitation method. In order to overcome the structural change due to oxygen desorption in the cathode active material with high nickel content, the physical and electrochemical analysis of the cathode active material according to the calcination temperature were investigated. Physical properties of $Li_{1.05}Ni_{0.9}Co_{0.05}Ti_{0.05}O_2$ were analyzed by FE-SEM, XRD and TGA. The electrochemical performance of the coin cell using a cathode active material and $LiPF_6$(EC:EMC=1:2 vol%) electrolyte was evaluated by the initial charge/discharge efficiency, cycle retention, and rate capabilities. As a result, the initial capacity and initial efficiency of cathode materials were excellent with 244.5~247.9 mAh/g and 84.2~85.8% at the calcination temperature range of $750{\sim}760^{\circ}C$. Also, the capacity retention exhibited high stability of 97.8~99.1% after 50cycles.

Production of Poly(Hydroxybutyric-Co-Hydroxyvaleric) Acid by Pseudomonas sp. HJ (Pseudomonas sp. HJ에 의한 Poly(Hydroxybutyric-Co-Hydroxyvaleric) Acid의 생산)

  • 손홍주;민관필이상준
    • KSBB Journal
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    • v.10 no.4
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    • pp.349-356
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    • 1995
  • To produce PHA(polyhydroxyalkanoic acid) from microbr, dozens of microorganism have been screened from sewage sludge. Selected a strain HJ out of 50 strains of PHA producing bacteria has a capability of accumulating large amounts of PHB/HV copolymer when grown in batch culture with a single carbon source (glucose) that was not generally considered as precursor of hydroxyvalerate monomer unit. The strain HJ was identified as the genus Pseudomonas with respect to morphological, cultural, and biochemical characteristics. The optimal temperature and pH for cell growth were $37^{\circ}C$ and 7.0. The optimal medium compositions for cell growth were glucose 1% as a carbon source, (NH4) 2SO4 0.2% as a nitrogen source, K2HPO4 0.3%, and KH2PO4 0.45%. TO investigate she optimal condition for PHA production two-step cultivation method was employed. PHA production was inducted by deficiency of NH4+, SO4-2, Mg+2. Besides carbon source, deficiency of all nutrients stimulated PHA productivity but deficiency of NH4+ stimulated the most HV monomer content. The highest PHA production was C/N molar ratio 95.2. Pseudomonas sp. HJ was also able to pyoduc PHB/HV copolymer when cultivated on alkane, alkanoate, alcohol as carbon sources. The contents of PHA and she proportions of hydroxyvalerate monomer units varied depending on the carbon sources. Especially Pseudomonas sp. HJ was able to incorporate hydroxyvalerate into PHB/HV to level as high as from 49 to 74 mol% when grown in a medium containing hexadecane and propionate. The purified PHA was identified PHB/HV copolymer by HNMR analysis.

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Fabrication and Characterization of UV-curable Conductive Transparent Film with Polyaniline Nanofibers (폴리아닐린 나노섬유를 이용한 광경화형 전도성 투명필름의 제조 및 특성)

  • Kim, Sung-Hyun;Song, Ki-Gook
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.531-535
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    • 2012
  • Conductive polyaniline (PANI) nanofibers in UV-curable resin were used for a transparent conductive film. The emeraldine-salt PANI (ES-PANI) nanofibers were prepared by chemical oxidation polymerization of aniline, which could be changed into emeraldine-base PANI by dedoping. EB-PANI nanofibers as a precursor for conductive fillers were thereby transformed into re-dpoed PANI (rES-PANI) by dodecylbenzenesulfonic acid in the UV-curable resin solution. rES-PANI nanofibers have high conductivity and long-term stability in the solution without a defect of nanostructure. The resulting conductive resin solution was proved to be highly stable where no precipitation of rES-PANI fillers was observed over a period of 3 months. The transparent film was spin-casted on a poly(methyl methacrylate) sheet of thickness ca. $5{\mu}m$. A surface resistance of $6.5{\times}10^8{\Omega}/sq$ and transmittance at 550 nm of 91.1% were obtained for the film prepared with a concentration of 1.4 wt% rES-PANI nanofibers in the solution. This transformation process of rES-PANI from ES-PANI by dedoping-redoping can be an alternative method for the preparation of an antistatic protection film with controllable surface resistance and optical transparencies with the PANI concentration in UV-curable solution.

Fabrication of Stack-Structured Gas Sensor of LaCrxCo1-xO3/Li1.3Al0.3Ti1.7(PO4)3 and Its NOx Sensing Properties (LaCrxCo1-xO3/Li1.3Al0.3Ti1.7(PO4)3의 적층구조를 가지는 가스센서 제조와 그의 NOx 검지특성)

  • Lee, Young-Sung;Shimizu, Y.;Song, Jeong-Hwan
    • Korean Journal of Materials Research
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    • v.25 no.8
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    • pp.423-428
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    • 2015
  • Impedancemetric $NO_x$ (NO and $NO_2$) gas sensors were designed with a stacked-layer structure and fabricated using $LaCr_xCo_{1-x}O_3$ (x = 0, 0.2, 0.5, 0.8 and 1) as the receptor material and $Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ plates as the solid-electrolyte transducer material. The $LaCr_xCo_{1-x}O_3$ layers were prepared with a polymeric precursor method that used ethylene glycol as the solvent, acetyl acetone as the chelating agent, and polyvinylpyrrolidone as the polymer additive. The effects of the Co concentration on the structural, morphological, and $NO_x$ sensing properties of the $LaCr_xCo_{1-x}O_3$ powders were investigated with powder X-ray diffraction, field emission scanning electron microscopy, and its response to 20~250 ppm of $NO_x$ at $400^{\circ}C$ (for 1 kHz and 0.5 V), respectively. When the as-prepared precursors were calcined at $700^{\circ}C$, only a single phase was detected, which corresponded to a perovskite-type structure. The XRD results showed that as the Co concentration of the $LaCr_xCo_{1-x}O_3$powders increased, the crystal structure was transformed from an orthorhombic phase to a rhombohedral phase. Moreover, the $LaCr_xCo_{1-x}O_3$ powders with $0{\leq}x<0.8$ had a rhombohedral symmetry. The size of the particles in the $LaCr_xCo_{1-x}O_3$powders increased from 0.1 to $0.5{\mu}m$ as the Co concentration increased. The sensing performance of the stack-structured $LaCr_xCo_{1-x}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensors was found to divide the impedance component between the resistance and capacitance. The response of these sensors to NO gas was more sensitive than that to $NO_2$ gas. Compared to other impedancemetric sensors, the $LaCr_{0.8}Co_{0.2}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensor exhibited good reversibility and reliable sensingresponse properties for $NO_x$ gases.

Simulation Analysis of Sludge Disposal and Volatile Fatty Acids Production from Gravity Pressure Reactor via Wet Air Oxidation (습식산화반응을 통한 중력식반응기로부터의 슬러지 처리 및 유기산 생산 공정모사)

  • Park, Gwon Woo;Seo, Tae Wan;Lee, Hong-Cheol;Hwang, In-Ju
    • Korean Chemical Engineering Research
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    • v.54 no.2
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    • pp.248-254
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    • 2016
  • Efficacious wastewater treatment is essential for increasing sewage sludge volume and implementing strict environmental regulations. The operation cost of sludge treatment amounts up to 50% of the total costs for wastewater treatment plants, therefore, an economical sludge destruction method is crucially needed. Amid several destruction methods, wet air oxidation (WAO) can efficiently treat wastewater containing organic pollutants. It can be used not only for sludge destruction but also for useful by-product production. Volatile fatty acids (VFAs), one of many byproducts, is considered to be an important precursor of biofuel and chemical materials. Its high reaction condition has instituted the study of gravity pressure reactor (GPR) for an economical process of WAO to reduce operation cost. Simulation of subcritical condition was conducted using Aspen Plus with predictive Soave-Redlich-Kwong (PSRK) equation of state. Conjointly, simulation analysis for GPR depth, oxidizer type, sludge flow rate and oxidizer injection position was carried out. At GPR depth of 1000m and flow rate of 2 ton/h, the conversion and yield of VFAs were 92.02% and 0.17g/g, respectively.

Ultrastructural Study on Development of the Superior Cervical Ganglion of Human Fetuses (인태아 상경신경절 발육에 관한 전자현미경적 연구)

  • Kim, Dae-Young;Kim, Baik-Yoon;Yoon, Jae-Rhyong
    • Applied Microscopy
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    • v.28 no.2
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    • pp.139-158
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    • 1998
  • The development of the superior cervical ganglion was studied by electron microscopic method in human fetuses ranging from 40 mm to 260 mm of crown-rump length (10 to 30 weeks of gestational age). At 40 mm fetus, the superior cervical ganglion was composed of clusters of undifferentiated cell, primitive neuroblast, primitive supporting cell, and unmyelinated fibers. At 70mm fetus, the neuroblasts and their processes were ensheated by the bodies or processes of satellite cells. The cytoplasm of the neuroblast contained rough endoplasmic reticulum, mitochondria, Golgi complex, Nissl bodies and dense-cored vesicles. As the neuroblasts grew and differentiated dense-cored vesicles moved away from perikaryal cytoplasm into developing processes. Synaptic contacts between the cholinergic axon and dendrites of postganglionic neuron and a few axosomatic synapses were first observed at 70 mm fetus. At 90 mm fetus the superior cervical ganglion consisted of neuroblasts, satellite cells, granule-containing cells, and unmyelinated nerve fibers. The ganglion cells increased somewhat in numbers and size by 150 mm fetus. Further differentiation resulted in the formation of young ganglion cells, whose cytoplasm was densely filled with cell organelles. During next prenatal stage up to 260 mm fetus, the cytoplasm of the ganglion cells contained except for large pigment granules, all intracytoplasmic structures which were also found in mature superior cervical ganglion. A great number of synaptic contact zones between the cholinergic preganglionic axon and the dendrites of the postganglionic neuron were observed and a few axosomatic synapses were also observed. Two morphological types of the granule-containing cells in the superior cervical ganglion were first identified at 90 mm fetus. Type I granule-containing cell occurred in solitary, whereas type II tended to appeared in clusters near the blood capillaries. Synaptic contacts were first found on the solitary granule-containing cell at 150 mm fetus. Synaptic contacts between the soma of type I granule-containing cells and preganglionic axon termials were observed. In addition, synaptic junctions between the processes of the granule- containing cells and dendrites of postganglionic neuron were also observed from 150 mm fetus onward. In conclusion, superior cervical ganglion cells and granule-containing cells arise from a common undifferentiated cell precursor of neural crest . The granule-containg cells exhibit a local modulatory feedback system in the superior cervical ganglion and nay serve as interneurons between the preganglionic and postganglionic cells.

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Formation of a MnSixOy barrier with Cu-Mn alloy film deposited using PEALD

  • Moon, Dae-Yong;Hwang, Chang-Mook;Park, Jong-Wan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.229-229
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    • 2010
  • With the scaling down of ultra large integrated circuits (ULSI) to the sub-50 nm technology node, the need for an ultra-thin, continuous and conformal diffusion barrier and Cu seed layer is increasing. However, diffusion barrier and Cu seed layer formation with a physical vapor deposition (PVD) method has become difficult as the technology node is reduced to 30 nm and beyond. Recent work on self-forming barrier processes using PVD Cu alloys have attracted great attention due to the capability of conformal ultra-thin barrier formation using a simple technique. However, as in the case of the conventional barrier and Cu seed layer, PVD of the Cu alloy seed layer will eventually encounter the difficulty in conformal deposition in narrow line trenches and via holes. Atomic layer deposition (ALD) has been known for its good step coverage and precise thickness control, and is a candidate technique for the formation of a thin conformal barrier layer and Cu seed layer. Conformal Cu-Mn seed layers were deposited by plasma enhanced atomic layer deposition (PEALD) at low temperature ($120^{\circ}C$), and the Mn content in the Cu-Mn alloys were controlled form 0 to approximately 10 atomic percent with various Mn precursor feeding times. Resistivity of the Cu-Mn alloy films decreased by annealing due to out-diffusion of Mn atoms. Out-diffused Mn atoms were segregated to the surface of the film and interface between a Cu-Mn alloy and $SiO_2$, resulting in self-formed $MnO_x$ and $MnSi_xO_y$, respectively. No inter-diffusion was observed between Cu and $SiO_2$ after annealing at $500^{\circ}C$ for 12 h, indicating an excellent diffusion barrier property of the $MnSi_xO_y$. The adhesion between Cu and $SiO_2$ was enhanced by the formation of $MnSi_xO_y$. Continuous and conductive Cu-Mn seed layers were deposited with PEALD into 32 nm $SiO_2$ trench, enabling a low temperature process, and the trench was perfectly filled using electrochemical plating (ECD) under conventional conditions. Thus, it is the resultant self-forming barrier process with PEALD Cu-Mn alloy film as a seed layer for plating Cu that has further potential to meet the requirement of the smaller than 30 nm node.

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