• Title/Summary/Keyword: Nickel reduction

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Synthesis and Characterization of New Polyaza Non-macrocyclic and Macrocyclic Nickel(II) Complexes Containing One 1,3-Diazacyclohexane Ring

  • Lee, Yun-Taek;Jang, Bo Woo;Kang, Shin-Geol
    • Bulletin of the Korean Chemical Society
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    • v.34 no.7
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    • pp.2125-2130
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    • 2013
  • A new nickel(II) complex $[NiL^1]^{2+}$ ($L^1$ = 1-(2-aminoethyl)-3-(N-{2-aminoethyl}aminomethyl-1,3-diazacyclohexane) containing one 1,3-diazacyclohexane ring has been prepared selectively by the metal-template condensation of formaldehyde with N-(2-aminoethyl)-1,3-propanediamine and ethylenediamine at room temperature. The complex reacts with nitroethane and formaldehyde to yield the pentaaza macrocyclic complex $[NiL^2]^{2+}$ ($L^2$ = 8-methyl-8-nitro-1,3,6,10,13-pentaazabicyclo[13.3.1]heptadecane) bearing one C-$NO_2$ pendant arm. The reduction of $[NiL^2]^{2+}$ by using Zn/HCl produces $[NiL^3(H_2O)]^{2+}$ ($L^3$ = 8-amino-8-methyl-1,3,6,10,13-pentaazabicyclo[13.3.1]heptadecane) bearing one coordinated C-$NH_2$ pendant arm that is readily protonated in acid solutions. The hexaaza macrocyclic complex $[NiL^4]^{2+}$ ($L^4$ = 8-phenylmethyl-8-nitro-1,3,6,8,10,13-hexaazabicyclo[13.3.1]heptadecane) bearing one N-$CH_2C_6H_5$ pendant arm has also been prepared by the reaction of $[NiL^1]^{2+}$ with benzylamine and formaldehyde. The nickel(II) complexes of $L^1$, $L^2$, and $L^4$ have square-planar coordination geometry in the solid states and in nitromethane. However, they exist as equilibrium mixtures of the square-planar $[NiL]^{2+}$ (L = $L^1$, $L^2$, or $L^4$) and octahedral $[NiL(S)_2]^{2+}$ species in various coordinating solvents (S); the proportion of the octahedral species $[NiL(S)_2]^{2+}$ is strongly influenced by the ligand structure and the nature of the solvent. Synthesis, spectra, and chemical properties of the nickel(II) complexes of $L^1-L^4$ are described.

Catalytic Effects and Characteristics of Ni-based Catalysts Supported on TiO2-SiO2 Xerogel

  • Jeong, Jong-Woo;Park, Jong-Hui;Choi, Sung-Woo;Lee, Kyung-Hee;Lee, Chang-Seop
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2288-2292
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    • 2007
  • The catalytic activities of nickel-based catalysts were estimated for oxidizing acetaldehyde of VOCs exhausted from industrial facilities. The catalysts were prepared by sol-gel methods of SiO2 and SiO2-TiO2 as a xerogel followed by impregnating Al2O3 powder with the nickel nitrate precursor. The crystalline structure and catalytic properties for the catalysts were investigated by use of BET surface area, X-ray diffraction (XRD), Xray photoelectron spectroscopy (XPS) and temperature programmed reduction (TPR) techniques. These results show that nickel oxide is transformed to NiAl2O4 spinel structure at the calcination temperature of 400 °C in response to the steps with after- and co-impregnation of Al2O3 powder in sol-gel process. The NiAl2O4 could suppress the oxidation reaction of acetaldehyde by catalysts. The NiO is better dispersed on SiO2-TiO2/Al2O3 support than SiO2/Al2O3 and SiO2-TiO2-Al2O3 supports. From the testing results of catalytic activities for oxidation of acetaldehyde, Catalysts showed a big difference in conversion efficiencies with the way of the preparation of catalysts and the loading weight of nickel. The catalyst of 8 wt.% Ni/TiO2-SiO2/Al2O3 showed the best conversion efficiency on acetaldehyde oxidation with 100% conversion efficiency at 350 °C.

Hydrophobic Self-assembled Monolayer(SAM) Coating for Enhanced Demolding Performance in Micromolding (마이크로몰딩의 이형성 향상을 위한 소수성 Self-assembled Monolayer(SAM) 코팅)

  • Park, Sang-Ha;Han, Seung-O;Park, Jong-Yeon;Mun, Seong-Uk;Park, Jeong-Ho
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.51 no.4
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    • pp.175-183
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    • 2002
  • In this paper, the surface modification effect of self-assembled monolayer(SAM) of 1-dodecanethiol [$CH_3$($CH_2$)$_{11}$SH] used as an anti-adhesive film in micromolding process was studied. Monolayers of 1-dodecanethiol[$CH_3$(CH$_2$)$_{11}$SH] were obtained by immersing a metal place in pure 1-dodecanethiol. SAM film on the nickel plate has been examined by using X-ray photoelectron spectroscopy(XPS). The focus has been placed on S-Ni bonding. From the XPS analysis, sulfur atoms were detected from the SAM film as a chemical composition of S-Ni. In order to measure an adhesion force of the SAM-coated nickel surface, atomic force microscopy(AFM) was used in force-distance mode, which whows the micro-adhesive force on solid surface. It was shown that adhesion forces measured from the SAM-coated nickel surface and the Ni surface without SAM coating were 3.52nN and 5.32nN, respectively. In order to investigate the effect of SAM coating on the surface foughness the replica in demolding process, hot embossing experiments were performed using a SAM-coated nickel master and a nickel master without SAM coating. Surface roughness of replica from the SAM-coated master showed 25nm and that of replica from master without SAM coating was 35nm. The smoother surface roughness of the replica from the SAM-coated, master is believed to result from reduction in the adhesion forces.ces.

Preparation of Ni-PTFE Electrode using Nickel Plating for Alkaline Fuel Cell (니켈도금기술을 이용만 알칼리형 연료전지용 Ni-PTFE전극의 개발)

  • Kim, Jae-Ho;Lee, Young-Seak
    • Transactions of the Korean hydrogen and new energy society
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    • v.20 no.4
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    • pp.291-299
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    • 2009
  • Ni-plated polytetrafluoroethylene(Ni-PTFE) particles($25{\mu}m$, $500{\mu}m$) were prepared by using nickel electroless plating. The Ni content in Ni-PTFE particles increased with increasing the amount of reduction agent. At about 53 wt% Ni content, $25{\mu}m$ Ni-PTFE particles showed conductivity of 320S/m. The Ni-PTFE particles were formed into the Ni-PTFE plate using heat treatment at $350^{\circ}C$ under $10{\sim}1000kg/cm^2$. The Ni-PTFE plate displayed the high conductivity of 5100S/m due to the formation of 3-dimentional Ni network. The plate was used as an electrode in an alkaline fuel cell(AFC). In terms of the current density, the Ni-PTFE electrode having higher Ni content(53 wt%) showed improved performance.

Effect of reaction factors on the characteristics of Ni-coating layer onto graphite (흑연표면의 니켈코팅층 특성에 미치는 반응인자의 영향)

  • Dong Jin Kim;Hun Saeong Chung;Myung Kyu Jung;Ki Byoung Youn
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.4
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    • pp.395-404
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    • 1994
  • Ni-graphite composite powders were prepared by reduction of $Ni^{++}$ from ammoniacal nickel sulfate solution on graphite core by hydrogen gas. Effect of reaction factors on the reduction rate and the properties of nickel layer were investigated by SEM, Optical Microscopy, size and chemical analysis. Induction period, a time lag between the injection of hydrogen gas and the start of the reduction, was 20~110 mins and affected by the reaction temperature and stirring speed. The reduction rate of $Ni^{++}$ was $4.5g/{\ell}/min$ at optimum condition and increased with increasing reaction temperature and stirring speed.

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Preparation and Characterization of Palladium Nanoparticles Supported on Nickel Hexacyanoferrate for Fuel Cell Application

  • Choi, Kwang-Hyun;Shokouhimehr, Mohammadreza;Kang, Yun Sik;Chung, Dong Young;Chung, Young-Hoon;Ahn, Minjeh;Sung, Yung-Eun
    • Bulletin of the Korean Chemical Society
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    • v.34 no.4
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    • pp.1195-1198
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    • 2013
  • Nickel hexacyanoferrate supported palladium nanoparticles (Pd-NiHCF NPs) were synthesized and studied for oxygen reduction reactions in direct methanol fuel cell. The NiHCF support was readily synthesized by a comixing of $Ni(OCOCH_3)_2$ and equimolar $K_3[Fe(CN)_6]$ solution into DI water under rigorous stirring. After the preparation of NiHCF support, Pd NPs were loaded on NiHCF via L-ascorbic acid reduction method at $80^{\circ}C$. Pd-NiHCF NPs were electrochemically active for oxygen reduction reaction in 0.1 M $HClO_4$ solution. X-ray absorption near edge structure analysis was conducted to measure the white line intensity of Pd-NiHCF to verify the OH adsorption. As a comparison, carbon supported Pd NPs exhibited same white line intensity. This study provides a general synthetic approach to easily load Pd NPs on porous coordination polymers such as NiHCF and can provide further light to load Pd based alloy NPs on NiHCF framework.

A Density-Functional Theory Study on Mechanisms of the Electrochemical Nitrogen Reduction Reaction on the Nickel(100) Surface (범밀도함수이론에 기초한 니켈(100) 표면에서의 전기화학적 질소환원반응 메커니즘에 관한 연구)

  • Minji Kim;Sangheon Lee
    • Korean Chemical Engineering Research
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    • v.61 no.4
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    • pp.604-610
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    • 2023
  • The nitrogen reduction reaction (NRR), which produces NH3 by reducing N2 under ambient conditions, is attracting attention as a promising technology that can reduce energy consumption in industrial processes. We investigated the adsorption behaviors at various active sites on the Ni (100) surface, which is widely used among catalytic metal surfaces capable of adsorbing and activating N2, based on density-functional theory calculations. We also investigated two N2 adsorption structures, so-called end-on and side-on structures. We find that for the end-on case, N2 is adsorbed on a top site, and the reaction proceeded in a distal pathway, while for the side-on case, N2 is adsorbed on a bridge site, and the reaction proceeded with enzymatic pathway. Finally, this study provides insight into the adsorption of metal catalyst surfaces for the NRR reactions based on the calculated Gibbs free energy profiles of the thermodynamically most favorable pathways.

Nanostructure Control of PtNiN/C Catalysts for Oxygen Reduction Reaction by Regulating Displacement Rate of Precursor (전구체 치환 속도 조절을 통한 산소환원반응용 PtNiN/C 촉매의 나노구조 제어)

  • Dong-gun Kim;Seongseop Kim;Sung Jong Yoo;Pil Kim
    • Clean Technology
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    • v.30 no.1
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    • pp.55-61
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    • 2024
  • Efforts are actively underway to address the issues related to the high cost of Pt-based catalysts for oxygen reduction reactions by designing high-performance Pt-based alloys through the control of their nanostructures. In this study, a method was proposed to control the nanostructure of Pt-based alloys, either hollow or core-shell, by adjusting the pH of the solution during the galvanic replacement reaction between the carbon-supported nickel-nickel nitride composite and the Pt ions. The physical characteristics, including the state, quantity, and morphology of the metal particles under different preparation conditions, were evaluated through X-ray diffraction, transmission electron microscopy, and inductively coupled plasma. When the prepared catalysts were employed for the oxygen reduction reaction, they exhibited an improvement in area specific-activity compared to a commercial Pt/C, with a 1.7 and 1.9-fold enhancement for the hollow and core-shell structured catalysts, respectively.

Characteristics of the Electrochemical Ion Exchanger for the Treatment of Cations in Nuclear Wastewater (원자력 폐수의 양이온 처리를 위한 전기화학적 이온교환체의 특성)

  • Hwang, Young-Gi
    • Journal of the Korean Society of Industry Convergence
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    • v.19 no.4
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    • pp.176-184
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    • 2016
  • Electrochemical ion exchange method is expected to be one of the most acceptable techniques for the separation of radioactive cations from nuclear wastewater. In this study a thin film of hexacyanoferrate on nickel surface was derivatized chemically in an aqueous potassium-ferricyanide solution. Electrochemical redox behavior of the nickel hexacyanoferrate(NiHCNFe) film electrode was investigated with the use of cyclic voltammetry potentiostated from -100 to 800 mV versus SCE. The electro-reduction characteristics of the NiHCNFe film were examined in the cobalt solutions. The NiHCNFe ion exchanger was more useful at lower concentration, lower temperature, and pH7 of the cobalt solution. The capacity loss of NiHCNFe was 0.018%/cycle that was less than the average loss of 2~3%/cycle of the convective organic exchanger. The 45~55% of the initial cobalt ions was electro-deposited on the NiHCNFe by using continuous recirculating reactor system. As a result, it was found that the electroactive NiHCNFe films showed better performance than the organic resins for the separation of cobalt ion from the aqueous solutions.