• 제목/요약/키워드: Ni-solution

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세자리 Schiff Base의 Ni(II) 착물의 분석 (Analysis of Tridentate Schiff Base Ni(II) Complex)

  • 채희남;최용국
    • 분석과학
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    • 제11권5호
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    • pp.332-340
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    • 1998
  • Salicylaldehyde와 2-hydroxy-1-naphthaldehyde를 2-aminophenol과 2-amino-p-cresol에 반응시켜 세자리 Schiff base 리간드($SIPH_2$, $SIPCH_2$, $HNIPH_2$, $HNIPCH_2$)들을 합성하였다. 이들 리간드를 Ni(II) 이온과 반응시켜 세자리 Schiff base Ni(II) 착물들을 합성 하였다. 이들 리간드와 그 착물들의 가상적인 구조와 특성을 원소분석, $^1H$-NMR, IR, UV-vis 분광법과 열 무게 분석법으로 알아보았다. Schiff base 리간드와 Ni(II) 착물의 몰비는 1:1로 결합하며, Ni(II)착물들은 3분자의 수화물이 배위된 6배위의 8면체 구조임을 알았다. 지지 전해질로서 0.1 M TBAP를 포함한 DMSO 용액에서 순환 전압전류법과 미분 펄스 전압전류법으로 세자리 Schiff base 리간드와 이들의 Ni(II) 착물들의 전기 화학적인 산화 환원 과정을 알아보았다. 세자리 Schiff base 리간드들의 전기 화학적 환원은 확산 지배적이고 비가역적으로 진행되었다. Ni(II) 착물의 전기화학적 환원과정은 1단계 1전자 반응으로 확산 지배적이고 준가역적으로 진행되었다. Ni(II) 착물들의 환원전위는 [$Ni(II)(HNIP)(H_2O)_3$]>[$Ni(II)(SIP)(H_2O)_3$]>[$Ni(II)(SIPC)(H_2O)_3$]>[$Ni(II)(HNIPC)(H_2O)_3$]순으로 양전위 방향으로 이동하였으며, 리간드의 영향은 크게 받지 않았다. 이들 결과로 부터 본 연구에서 합성한 Ni(II)착물은 [$Ni(II)(HNIPC)(H_2O)_3$] 착물이 DMSO용매에서 가장 안정함을 알 수 있다.

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음향화학법으로 니켈을 코팅한 알루미나의 제조 및 분석 (Preparation and analysis of nickel-coated alumina by sonochemistry)

  • 김진우;최성우;이창섭
    • 분석과학
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    • 제24권2호
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    • pp.61-68
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    • 2011
  • 알루미나에 니켈을 코팅하는 효율을 높이기 위하여 졸-겔법을 이용하여 비결정성 알루미나를 제조한 후, 음향화학법을 이용하여 니켈을 알루미나에 코팅하여 미립자를 제조하였다. 니켈을 코팅한 알루미나 미립자는 여러 가지 소성온도($500^{\circ}C$, $1,000^{\circ}C$), 니켈용액의 농도(0.01 M~0.2 M), 초음파반응시간 (30 min, 2 h)의 조건에서 제조하였다. 제조한 미분체는 X-Ray Diffractometer (XRD), Scanning Electron Microscope (SEM), Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES), Particle Size Analyzer (PSA)로 특성을 분석하였다. 니켈용액의 농도가 진해짐에 따라 그리고 초음파반응시간이 길수록 니켈의 코팅량이 증가하였다. 알루미나에 니켈을 코팅하는데 있어 $1000^{\circ}C$의 소성온도, 0.1 M의 니켈용액의 농도, 2시간의 초음파에 반응하였을 때 알루미나에 니켈이 가장 많이 코팅되었다. 그리고 평균입자의 크기는 835.9~986.7 nm였다.

수소제조를 위한 다공성 FeCrAl 금속 합금 Foam의 NiO 촉매 담지 및 미세구조 분석 (Synthesis and Microstructure Analysis of NiO Catalysts Coated on the FeCrAl Metal Alloy Foam for Hydrogen Production)

  • 이유진;안건형;박만호;이창우;최상현;정주용;조성종;이근재;안효진
    • 한국재료학회지
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    • 제24권8호
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    • pp.393-400
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    • 2014
  • NiO catalysts were successfully coated onto FeCrAl metal alloy foam as a catalyst support via a dip-coating method. To demonstrate the optimum amount of NiO catalyst on the FeCrAl metal alloy foam, the molar concentration of the Ni precursor in a coating solution was controlled, with five different amounts of 0.4 M, 0.6 M, 0.8 M, 1.0 M, and 1.2 M for a dip-coating process. The structural, morphological, and chemical bonding properties of the NiO-catalyst-coated FeCrAl metal alloy foam samples were assessed by means of field-emission scanning electron microscopy(FESEM), scanning electron microscopy-energy dispersive spectroscopy(SEM-EDS), X-ray diffraction(XRD), and X-ray photoelectron spectroscopy(XPS). In particular, when the FeCrAl metal alloy foam samples were coated using a coating solution with a 0.8 M Ni precursor, well-dispersed NiO catalysts on the FeCrAl metal alloy foam compared to the other samples were confirmed. Also, the XPS results exhibited the chemical bonding states of the NiO phases and the FeCrAl metal alloy foam. The results showed that a dip-coating method is one of best ways to coat well-dispersed NiO catalysts onto FeCrAl metal alloy foam.

무전해 Ni-P 도금의 공정조건에 따른 도금피막 특성변화 (Electroless Ni-P layer Characteristics in accordance with the plating process conditions)

  • 이홍기;전준미;박해덕
    • 한국표면공학회지
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    • 제36권3호
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    • pp.263-271
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    • 2003
  • Optimal conditions of electroless nickel plating in acid baths has been studied for industrial applications of a developed EN solution. The phosphorus content in the deposition ranges from 8 to $12\;wt.\%$. The investigated EN plating parameters are ion concentrations of nickel and hypophosphite, concentration of reducing and complexing agent, temperature, and pH. The average plating rate of Ni-P deposition was ca. $14{\mu}m/h$. The EN solution used shows a deposition rate of $10{\mu}m/h$ up to seven metal turnovers.

전기도금법으로 제조한 Ni-Fe 나노박막의 스트레스와 자기적 특성에 미치는 용액의 조건 및 전류밀도의 영향 (Effect of Bath Conditions and Current Density on Stress and Magnetic Properties of Ni-Fe Nano Thin Films Synthesized by Electrodeposition Methods)

  • 구본급
    • 한국표면공학회지
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    • 제44권4호
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    • pp.137-143
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    • 2011
  • The internal stress and magnetic properties (coercivity and squareness) of Ni-Fe nano thin film synthesized by electrodeposition method were studied as a function of acidic chloride bath conditions (composition and temperature) and current density. Fe deposition patterns were different depending on the temperature of the solution, the stress of film decreased with increasing the solution temperature, and the depending on the amount of Fe deposition showed a parabolic shape. The grain size of film was inversely proportional to stress of thin film. The internal stress of thin film and magnetic properties were deeply relevant, and the stress of thin film had a relationship with bath conditions and grain size of the thin film surface.

Synthesis, Structural and Electrical Characterizations of $Pr_{2-x}Ba_xNiO_{4{\pm}\delta}{^\$}$

  • 장영기;권영구;변송호
    • Bulletin of the Korean Chemical Society
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    • 제16권2호
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    • pp.120-125
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    • 1995
  • Solid solutions of Pr2-xBaxNiO4±δ with K2NiF4-type structure were prepared in air and characterized by powder X-ray diffraction, Rietveld refinements, iodometry titrations, and conductivity measurements. The range of the solid solution was 0 ≤ x < 0.5. The crystal structure changes from orthorhombic (Fmmm) for x ≤ 0.1 to pseudo-tetragonal (I4/mmm) for x ≥ 0.2. The orthorhombic structure of x=0.1 transforms to tetragonal at low temperature. The bond distances obtained from the Rietvel analyses did not vary significantly with the Ba content except that of Ni-O (parallel to the c-axis) which showed an abrupt increase from x=0.1 to 0.2. The excess oxygen content (δ) decreases from 0.241 to 0.03 with increasing substituted Ba contents within the solution range. The samples are all semiconductors at the temperature range 4 < T < 300 K.

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

  • 황영기
    • 한국산업융합학회 논문집
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    • 제19권4호
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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.

Self-Assembled and Alternative Porphyrin-Phthalocyanine Array

  • Kwag, Gwang-Hoon;Park, Eun-Joo;Kim, Sung-Hyun
    • Bulletin of the Korean Chemical Society
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    • 제25권2호
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    • pp.298-300
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    • 2004
  • An alternative molecular porphyrin-phthalocyanine aggregate was prepared and characterized with UV-visible and X-ray absorption spectroscopies. UV-visible experiments evidence 1-dimensional porphyrin-phthalo-cyanine array formed by mixing $SnTPPCl_2 ({\lambda}_{max}=429,\;{\varepsilon}=2.4{\times10^ 5 /M{\cdot}cm)\;and\;NiPc(OBu)_8({\lambda}_{max}=744 nm,\;{\varepsilon}= 2.0{\times}10^ 5 /M{\cdot}cm)$ in solution. In the UV-visible spectrum of the porphyrin-phthalocyanine array, $(SnPNiPc)_n$, a new Q-band appeared at 844 nm with decrease of the Q-band peak of $NiPc(OBu)_8$ at 744 nm. The red-shift of Q-band evidences an alternative porphyrin-phthalocyanine array formed in solution through metal-halide interaction rather than ${\pi}-{\pi}$ facial interaction, in which nickel of $NiPc(OBu)_8$ coordinates with chloride of $SnTPPCl_2$ through self assembly. Ni K-edge XANES (X-ray absorption near edge structure) spectra also support the axial ligation of nickel to chloride. The square planar structure of $NiPc(OBu)_8$ turns to an octahedral structure in (SnPNiPcSnP) by axial ligation. A higher energy-shift (0.2 eV) of the preedge peak of (SnPNiPcSnP) indicaties partial oxidation of nickel by charge transfer from NiPc$(OBu)_8$ to SnTPPCl$_2$.

무전해도금에 의한 Ni-Tl-P 피막형성에 관한 연구 (A Study on Formation of Ni-Tl-P deposits by Electroless Plating)

  • 류일광;추현식
    • 한국표면공학회지
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    • 제33권2호
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    • pp.126-134
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    • 2000
  • This study investigated the bath compositions and plating conditions and crystal structure used for achieving nickel-thallium-phosphorus deposits by means electroless plating. The electroless nickel-thallium-phosphorus deposits were achieved with a bath using sodium hypophosphite as the reducing agent and sodium citrate as the complexing agent. The depositing rate was 10.5mg.$cm^{2-1}$ .$hr^{-1 }$ from the optimistic bath composition, 0.1M nickel sulfate, 0.005M thallium sulfate, 0.2M sodium hypophosphite, and 0.05M sodium citrat and the recommended plating conditions, pH 5.5 and $90^{\circ}C$. The composition of alloy deposits determined by X-ray analysis (EDS) that the Thallium was increased with major increasing concentration of complexing agent and thallium ion in bath solution, it decreased according to the increasing concentrations of reduction agent in the bath solution, Bit Phosphorus showed a contrary to the thallium. It was observed from X-ray diffraction analysis, Scanning Electron Microscopy and Transmission Electron Microscopy. The crystalline structure of deposits was amorphous at the first deposited state but it was changed $Ni-T1-Ni_{5}$ $P_2$ polycrystalline when subjected to 1 hour heat treatment of more than $350^{\circ}C$. TEM observation demonstrated that the microstructure was identical to the result of the XRD at as deposited but it became $Ni-Tl-Ni_{5}$ $P_2$ polycrystalline when heated. And grain size was 10-50nm.

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분말 모합금 빌렛으로부터 제조된 Ni-W 합금테이프의 기계적 성질과 집합도 (Texture and Mechanical Properties of Ni-W Alloy Tapes Fabricated from Powder Mother Billets)

  • 김민우;전병혁;지봉기;정규동;김찬중
    • 한국분말재료학회지
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    • 제14권1호
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    • pp.13-18
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    • 2007
  • The mother Ni-W (1-5 wt.%) alloy billets for coated conductor substrate were fabricated by powder metallurgy process. The tensile test results for the sintered Ni-W rods showed the increase of mechanical strength and decrease of ductility with increasing W content due to the solid solution hardening. All the fracture surfaces of the tested specimens showed the typical ductile fracture mode of dimple rupture due to the local necking. The Ni-W alloy billets were made into tape by cold rolling. After the appropriate heat treatment for recrystallization, the brass texture formed by the cold rolling was converted to the complete cube texture. The in-plane and out of plane texture of the tapes estimated by x-ray pole figure were smaller than 9 degree and 7 degree, respectively. The effect of the W addition on the texture development seems not to be significant.