• Korean Chemical Engineering Research
• /
• v.59 no.2
• /
• pp.281-295
• /
• 2021

In this study, the direct amination of ethanol was performed over impregnated Ni on SiO2-Al2O3 mixed oxide catalysts prepared by varying Si/(Si + Al) molar ratio to 30 mol%. To characterize the physico-chemical properties of the catalysts used, X-ray diffraction (XRD), N2-physisorption, temperature-programmed desorption of iso-propyl alcohol (IPA-TPD), temperature-programmed desorption of ethanol (EtOH-TPD), temperature-programmed reduction with H2 (H2-TPR), H2-chemisorption and transmission electron microscopy (TEM) were used. The acidic property was continuously increased until Si/(Si + Al) = 30 mol% in SiO2-Al2O3 mixed oxides used. The dispersion of Ni metal and surface area, acid characteristics of the supported Ni catalyst have a complex effect on the catalytic reaction activity. The low reduction temperature of nickel oxide and acidic properties were beneficial to the formation of acetonitrile. In terms of conversion of ethanol, Ni/SiO2-Al2O3 catalyst with a molar ratio of 10 mol% Si/(Si+Al) showed the highest activity and a volcanic curve based on it. The tendency of results were consistent in the metal dispersion and catalytic activity.

• Transactions of the Korean hydrogen and new energy society
• /
• v.19 no.1
• /
• pp.18-25
• /
• 2008

The membrane electrode assembly(MEA) was prepared by a nonequilibrium impregnation- reduction (I-R) method. Nafion 117 and covalently cross-linked sulfonated polyetherether with tungsto- phosphoric acid (CL-SPEEK/TPA30) prepared by our laboratory, were chosen as polymer electrolyte membrane(PEM). $Pt(NH_3)_4Cl_2$, $RuCl_3$ and reducing agent $(NaBH_4)$ were used as electrocatalytic materials. Electrochemical activity surface area(ESA) and specific surface area(SSA) of Pt cathodic electrode with Nafion 117 were $22.48m^2/g$ and $23.50m^2/g$ respectively under the condition of 0.8 M $NaBH_4$. But Pt electrode prepared by CL-SPEEK/TPA30 membrane exhibited higher ESA $23.46m^2/g$ than that of Nafion 117. In case of Pt-Ru anodic electrode, the higher concentration of Ru was, the lower potential of oxygen reduction and region of hydrogen desorption was, and Pt-Ru electrode using 10 mM $RuCl_3$ showed best properties of SSA $34.09m^2/g$ with Nafion 117. In water electrolysis performance, the cell voltage of Pt/PEM/Pt-Ru MEA with Nafion 117 showed cell property of 1.75 V at $1A/cm^2$ and $80{\circ}C$. On the same condition, the cell voltage with CL-SPEEK/TPA30 was the best of 1.73 V at $1A/cm^2$.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 2001.11a
• /
• pp.30-30
• /
• 2001

$Bi_2Te_3$계 열전재료는 200~400K 정도의 저온에서 네어지 변환효율이 가장 높은 재료로써 열전냉각, 바런재로 등에 응요하기 위하여ㅠ 제조법 및 특서에 관한 많은 연구가 진행되어 왔다. $Bi_2Te_3$계 화합물은 rhombohedral의 결정 구조를 가지는 층상 화 ;물로 결정대칭성으로 인해 연전기적으로 큰 이방성을 나타낸다. 현재는 일반향용고법에 의해서 입자를 a축 방향으로 성장시켜 큰 결정립을 가진 다결정재료를 사용하고 있으나, c면이 매우 취약하기 때문에 가공서이 나쁘다. 따라서 이와같은 단점을 개선하기 위하여 기계적 강도를 높일 수 있는 가공공정 및 합금설계에 대한 연구가 활발히 진행되고 있다. 측히 열간 압출법으로 제조된 열전재료는 결정립의 미세화와 높은 이방성으로 성능지수와 기계적 강도를 향상시킬 수 있다는 연구결과가 보고되고 있다 또한 Schultz드의 연구결과에 의하면 $Bi_2Te_3$ 계 열전재료는 소성변형에 의하여 발생한 점결함에 의하여 캐리어 농도가 변화되며 이로 인하여 재료의 전기적 성질이 결정된다고 하였다. 따라서 상당히 큰 소성가공량과 열전측성과의 관계를 규명하는 것은 매우 중요하다. 이에 본 연구에서는 압출변수 중 소성가공량에 중요한 변수로 작요아는 압출비를 변화시켜 최적의 열간 소성가공량을 검토하고, 이에 따른 열전측성과 압출비와의 상관관계에 대하여 연구하는 것을 목적으로 하였다. 연구에 사용된 N형의 조성은$Bi_2Te_{2.75}Se_{0.15}$로서 순도 99.99를 사용하였고, dopant로 0.1wt%의 $SbI_3$를 사용하였다. $Bi_2Te_{2.75}Se_{0.15}$ 분말은 가스분사법(Gas atomization Process)를 이용하여, 용탕제조시 아르곤가스로 산화를 방지하였고, 냉매로는 질소가스를 이용하였다. 제조된 분말을 기ㅖ적 분급법을 이용하여 분급하였고, 냉매로는 질소가스를 이용하였다. 제조된 분말을 기계적 분급ㅂ법을 이용하여 분급하였고, 압출에 이용된 분말은 250$\mu\textrm{m}$이하의 크기를 사용하였다. 또한 분말제조과정 중 형성되는 표면산화층을 제거하기 위하여 36$0^{\circ}C$에서 4시간동안 수소 환원처리를 행하였다. 제조된 분말은 열간 압출을 위하여 Aㅣcan에 넣고 냉간성형체를 만들고, 진공처리를 한 후 밀봉하여 탈가스처리를 하였다. 압출다이는 압출비가 각각 28:1과 16:1인 평다이(9$0^{\circ}C$)를 사용하여 각각 내경이 9, 12cm이고, 길이가 50, 30cm인 압출재를 제조하였다. 열간압출한 후의 미세조직을 광학현미경으로 압출방향에 평행한 방향과 수직방향으로 관찰하였고, 열간 압출재 이방성을 검토하기 위하여 X선 회절분석을 실실하여 결정방위를 확인하였다. 전기 비저항 및 Seebeck 계수 측정을 위하여 각각 2$\times$2$\times$10$mm^3$ 그리고 5$\times$5$\times$10$mm^3$ 크기의 시편을 준비하였다.준비하였다.

• Nuclear Engineering and Technology
• /
• v.13 no.3
• /
• pp.145-152
• /
• 1981

Even though a lately reported method of high temperature exchange labelling of o-iodo-hippuric acid (Hippuran) in the absence of oxidizing agent was considered to be an attractive one, the exchange mechanism was somewhat unclear. In this study iodine isotope exchanges between o-iodohippuric acid (OIH) and radioiodide ($^{125}$ $I^{ }$) or between OIH and molecular radioiodine ($^{125}$ $I_2$) were carried out at two different temperatures. Rate constants and activation parameters were measured by applying a radio-paper chromatography technique. Since o-iodobenzoic acid is known as a by-product in the exchange labelling of OIH, data were also obtained for the OIB-iodide systems for comparison. The rate constant was increased in the order of OIB...$^{125}$ $I^{[-10]}$ >OIB...$^{125}$ $I_2$>OIH..$^{125}$ $I^{[-10]}$ >OIH...$^{125}$ $I_2$ and the activation parameters for OIH were generally larger than those for OIB :$\Delta$H$\neq$$_{OIH}$>$\Delta$H$\neq$$_{OIB}$, $\Delta$S$\neq$$_{OIH}$>$\Delta$S$\neq$$_{OIB}$. These results suggest that the mechanism of the high temperature exchange is predominantly nucleophilic even though some electrophilic character can also be involved depending upon reaction conditions. Such a fact may well be caused by a feasible formation of hydrogen bonding type transition state due probably to the ortho substituent effect of-CONHC $H_2$COOH. Thus, the high temperature exchange method is estimated to be quite effective for labelling Hippuran especially at a small research center where reducing agent-free $^{131}$ I is unavailable.ailable..

• Clean Technology
• /
• v.13 no.1 s.36
• /
• pp.54-63
• /
• 2007

Even traces of CO in the hydrogen-rich feed gas to proton exchange membrane fuel cells (PEMFC) poison the platinum anode electrode and dramatically decrease the power output. In this work, a variety of catalytic materials consisting of $Cu/Ce_xZr_{1-x}O_2$, (x = 0.0-1.0) were synthesised, characterized and tested for CO oxidation and preferential oxidation of CO (PROX). These catalysts prepared by hydrothermal and deposition-precipitation methods. The catalysts were characterized by XRD, XRF, SEM, BET, $N_2O$ titration and oxygen storage capacity (OSC) measurement. The effects of composition of the support and degree of excess oxygen were investigated fur activity and $CO_2$ selectivity with different temperatures. The composition of the support markedly influenced the PROX activity. Among the various $Cu/Ce_xZr_{1-x}O_2$ catalysts having different composition, $Cu/Ce_{0.9}Zr_{0.1}O_2$ and $Cu/Ce_{0.7}Zr_{0.3}O_2$ showed the highest activities (>99%) and selectivities (ca.50%) in the temperature range of $150{\sim}160^{\circ}C$. It was found that by using of $Ce_xZr_{1-x}O_2$ mixed oxide support which possesses a high oxygen storage capacity, oxidation-reduction activity of Cu-based catalyst was improved, which resulted in the increase of catalytic activity and selectivity of CO oxidation in excess $H_2$ environments.

• Clean Technology
• /
• v.17 no.2
• /
• pp.166-174
• /
• 2011

The xAl-yCe oxide catalysts with different mol ratios of Al/(Al+Ce) were prepared by a co-precipitation method and Pt supported on xAl-yCe oxide catalysts were synthesized by an incipient wetness impregnation method. The catalysts were characterized by X-ray Diffraction (XRD), $N_2$ sorption, and $H_2$/CO-temperature programmed reduction ($H_2$/CO-TPR) to correlate with catalytic activities in co oxidation. Among the catalysts studied here, Pt/1Al-9Ce oxide catalyst showed the highest activity in dry and wet reaction conditions and the catalytic activity showed a typical volcano-shape curve with respect to Al/(Al+Ce) mol ratio. When the presence of 5% water vapor in the feed, the temperature of $T_{50%}$ was shifted ca. $30^{\circ}C$ to lower temperature region than that in dry condition. From CO-TPR, the desorption peak of $CO_2$ on Pt/1Al-9Ce oxide catalyst showed the highest value and well correlated the catalytic performance. It indicates that the Pt/1Al-9Ce oxide catalyst has a large amount of active sites which can be adsorbed by co and easy to supplies the needed oxygen. In addition, the amount of pentacoordinated $Al^{3+}$ sites obtained through $^{27}Al$ NMR analysis is well correlated the catalytic performance.

• Journal of Advanced Marine Engineering and Technology
• /
• v.41 no.3
• /
• pp.230-237
• /
• 2017

In this study, electrochemical methods were used to determine the optimum protection potential of S355ML steel for the cathodic protection of offshore wind-turbine-tower substructures. The results of potentiodynamic polarization experiments indicated that the anodic polarization curve did not represent a passivation behavior, while under the cathodic polarization concentration, polarization was observed due to the reduction of dissolved oxygen, followed by activation polarization by hydrogen evolution as the potential shifted towards the active direction. The concentration polarization region was found to be located between approximately -0.72 V and -1.0 V, and this potential range is considered to be the potential range for cathodic protection using the impressed current cathodic protection method. The results of the potentiostatic experiments at various potentials revealed that varying current density tended to become stable with time. Surface characterization after the potentiostatic experiment for 1200 s, by using a scanning electron microscope and a 3D analysis microscope confirmed that corrosion damage occurred as a result of anodic dissolution under an anodic polarization potential range of 0 to -0.50 V, which corresponds to anodic polarization. Under potentials corresponding to cathodic polarization, however, a relatively intact surface was observed with the formation of calcareous deposits. As a result, the potential range between -0.8 V and -1.0 V, which corresponds to the concentration polarization region, was determined to be the optimum potential region for impressed current cathodic protection of S355ML steel.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2014.02a
• /
• pp.427-428
• /
• 2014

서론: 최근 전세계적인 고령화 진행에 따른 뇌졸중, 파킨슨병, 알츠하이머병 등과 같은 각종 뇌관련 질환에 대한 관심이 더욱 높아지고 있으며 다양한 뇌질환 치료를 위하여 뇌 신경 신호의 정확한 검출 대한 연구가 학계에서 활발히 진행되고 있다. 효과적인 뇌 신경 신호 검출을 위해서는 세포조직의 손상을 최소화 할 수 있는 초소형 신경탐침 및 극소 면적내에서 극대화된 검출 전극이 구현되어야 한다. 그러나, 극소 면적내에 구성된 소면적 전극을 통한 신호 검출은 전극 계면에서의 높은 임피던스를 야기시켜 정밀한 신경신호 검출에 어려움을 만든다. 따라서, 뇌 신경 신호 검출시 전극 계면에서의 낮은 임피던스를 검출하기 위한 다결정실리콘, 이리듐 산화막, 탄소나노튜브와 같은 다양한 전극 소재를 이용한 신경탐침 연구가 제안되어 왔다. 본 연구에서는 극소화된 전극면적과 신경세포 계면에서의 저 임피던스 신경신호 검출을 위하여 비이온성 계면활성제와 전해도금을 이용하여 높은 거칠기값을 갖는 나노동공 백금층을 검출 전극으로 활용하였다. 실험 결과: 제작된 신경탐침의 몸체는 실리콘으로 이루어지며, 탐침 끝단에는 신호 측정을 위한 나노동공 백금층을 갖는 전극들이 집적되어 있다. Fig. 1 는 제작된 나노동공 백금을 갖는 신경탐침의 이미지 (a), SEM (b), TEM (c), FESEM (d) 측정결과를 보여준다. 0.9 %의 NaCl 용액에서 제작된 신경탐침의 계면임피던스 및 위상각 변화에 대한 측정결과가 Fig. 2에 나타나 있다. 1.2 kHz 주파수에서 $942.6K{\Omega}$ ($0.029{\Omega}cm^2$, $3.14{\mu}m^2$)로 극대화된 실표면적을 갖는 나노동공 백금층에 의하여 매우 낮은 임피던스 특성을 보인 것으로 판단된다. 또한 제작된 신경탐침은 위상각이 $-82.9^{\circ}$로서 캐패시터와 같은 역할을 하고 있다고 예상할 수 있었으며 $4.6mFcm^{-2}$의 축전용량값을 보였다. Fig. 3는 1 M의 황산용액에서 나노동공백금층이 형성된 신경탐침 전극과 형성 전의 전기화학적 표면변화를 비교분석한 결과로서 나노동공 백금층의 형성 전/후의 전류응답 특성이 상이하게 나타났다. 나노동공 백금층의 실표면적 극대화로 인한 전류응답수치 또한 크게 향상 되었으며, 0~-0.25 V 영역에서의 수소 흡착에 따른 환원곡선은 전형적인 백금 특성을 보여주는 결과로 판단 할 수 있다. Table 1는 기존에 연구되었던 신경탐침들과 본 연구에서 제작된 나노동공 백금을 갖는 신경탐침의 임피던스와 캐패시턴스 특성을 비교한 결과이다. 결론: 본 연구에서는 실리콘 신경탐침 끝단에 집적된 전극상에 전해도금법을 이용하여 높은 거칠기값을 갖는 나노동공 백금층을 형성하고 전극 계면상의 낮은 임피던스를 검출을 하였다. 나노동공 백금층을 갖는 신경탐침은 순환전압전류법을 통해 극대화된 실표면적을 극대화를 확인할 수 있었으며, 극대화된 검출 전극면은 저 임피던스 측정에 용이함을 실험을 통해서 증명할 수 있었다. 따라서, 높은 거칠기값의 나노동공 백금층은 초소형화된 신경탐침상에 집적되는 전극면적소형화와 다수의 전극 구현에 효과적일 것으로 판단되며 보다 정확한 신경신호 검출을 통한 뇌질환의 명확한 이해에 유망할 것으로 판단된다.

• Clean Technology
• /
• v.21 no.1
• /
• pp.68-75
• /
• 2015

In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl₂O₄@Al micro-composite for heterogeneous catalysts support. The CoAl₂O₄@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl₂O₄ shell. For comparison, CoAl₂O₄ was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl₂O₄@Al and CoAl₂O₄ were prepared by incipient wetness impregnation and characterized by N₂ adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl₂O₄@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl₂O₄ due to facilitated heat transport through the core-shell structure. The CoAl₂O₄@Al and CoAl₂O₄ also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl₂O₄@Al core-shell than CoAl₂O₄. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.

• Korean Journal of Materials Research
• /
• v.10 no.1
• /
• pp.97-106
• /
• 2000

In these respects the purpose of this research is manufacturing Co-W-P alloy thin film on the corning glass 2948 by electroless plating method using $NaH_2PO_2H_2O$ (sodium hypophosphite) as a reductant, and analyzing deposition rate, alloy composition, microstructure, and magnetic characteristics at various pH's and temperatures. For Co-P alloy thin film, the reductive deposition reaction occurred only in basic condition, not in acidic condition. The deposition rate increased as the pH and temperature increased, and the optimum condition was found at the pH of 10 and the temperature of 8$0^{\circ}C$. Also magnetic characteristics was found to be most excellent at the pH of 9 and the temperature of 7$0^{\circ}C$, resulting in the coercive force of 870Oe and the squareness of 0.78. At this condition, the contents of P was 2.54% and the thickness of the film was 0.216$\mu\textrm{m}$. For crystal orientation, we could not observe fcc for $\beta$-Co. On the other hand, (1010), (0002), (1011) orientation of hcp for $\alpha$-Co was observed. We could confirm the formation of longitudinal magnetization from dominant (1010) and (1011) orientation of Co-P alloy. For Co-W-P alloy thin film, coercive force was 500Oe and squareness was 0.6. For crystal orientation, (0002) orientation of $\alpha$-Co was dominatly found. Then we could confirm the formation of perpendicular magnetization. The content of P was constant at 0.8$\pm$0.2% and the content of W increased as the concentration of Na$_2$WO$_4$increased. When the concentration of Na$_2$WO$_4$was 0.1mol/L, the composition of W was 20%. We observed the changes of magnetic characteristics and microstructure of thin film depositions of Co-W-P by the heat treatment. For heat treatment, the temperature was increased step by step to 10$0^{\circ}C$, 20$0^{\circ}C$, 30$0^{\circ}C$, and 40$0^{\circ}C$ and it took 1 hour at each step in the reductive condition of hydrogen gas. By the heat treatment, flatness of surface was improved, but there were no changes on the magnetic characteristics and the microstructures.