• 한국재료학회:학술대회논문집
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• 한국재료학회 2000년도 추계학술발표강연 및 논문개요집
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• pp.155-155
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• 2000

• 공업화학
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• 제24권4호
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• pp.438-442
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• 2013

본 연구에서는 무전해 도금법으로 니켈과 인을 탄소섬유 표면에 코팅한 후, 열처리시키는 과정에서 일어나는 변화를 다양한 분석방법을 이용하여 연구하였다. 전자현미경(Scanning Electron Microscopy, SEM)을 이용한 연구에서는, 코팅 후 추가적인 열처리를 하지 않은 경우 평평한 표면구조를 관찰하였으나, 열처리 온도가 $350^{\circ}C$에 이르면서 다공성구조가 생성됨을 알았다. 열처리 온도를 $50^{\circ}C$ 간격으로 증가시키면서 연구한 결과 $650^{\circ}C$까지는 열처리 온도가 증가할수록 기공의 크기는 증가하고, 개수는 감소하는 경향성이 관찰되었다. X-선 회절법(x-ray diffraction, XRD) 측정 결과, 코팅 후 추가 열처리가 없는 경우 금속성 Ni, Ni-P 화합물이 관찰되었으며, 열처리 온도가 증가함에 따라 NiO 봉우리는 세기가 증가하며, 금속성 Ni 봉우리의 세기는 감소하였다. X-선 광전자 분광법(X-ray Photoelectron Spectroscopy, XPS) 측정에서는 $650^{\circ}C$, $700^{\circ}C$의 열처리 후 인 산화물이 표면에서 검출됨을 확인하였는데, 이는 코팅된 니켈 필름의 내부에 존재하던 인 화합물이 열처리 온도가 증가함에 따라서 표면 밖으로 빠져 나오는 현상이 일어나는 결과로 해석할 수 있다. 이상의 분석 데이터를 토대로, 무전해 도금으로 코팅된 Ni-P 화합물($Ni_xP_y$)이 열처리 과정에서 산화되면서, 이때 생성된 인 화합물 기체가 승화하면서 필름에 기공을 생성시키는 것으로 제안할 수 있다. 다공성 물질은 넓은 비표면적 등의 우수한 물성때문에 불균일 촉매 등 다양한 분야에 적용될 수 있으며, 본 연구에서 소개하는 다공성 니켈 필름의 제작법은 대량 생산에 적용이 쉬워 환경 필터 분야 등의 다양한 곳에 응용될 수 있을 것으로 생각된다.

• 한국재료학회지
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• 제11권8호
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• pp.661-665
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• 2001

$\sigma$-VFe 금속간화합물에 대한 기계적 합금화(MA) 효과를 중성자 및 X선 회절법으로 조사하였다. MA 분말의 구조분석은 X선 회절(Cu-K$\alpha$) 린 중성자회절(HRPD, λ=1.835$\AA$)을 이용하여 행하였다. $\sigma$-VFe화합물의 MA시 큰 구조변화가 관찰되었으며, MA 60시간의 경우 Fe-Fe 훤자분포는 unit cell에 30개의 원자를 포함하고 있는 $\sigma$상의 tetragonal구조에서 $120^{\circ}C$이상에서 안정하게 존재하는 $\alpha$-(V,Fe) 고용체의 bcc 구조로 상변화함을 알 수 있었다. 또한 $\alpha$-VFe 화합물에 대한 중성자 및 X선 회절패턴의 비교분석을 행하였으며 그 결과 $\sigma$상이 가지는 화학적 규칙성에 기인하는 (101)과 (111) 회절 피크가 중성자 회절에서 뚜렷하게 관찰됨을 알 수 있었다.

• 분석과학
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• 제13권2호
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• pp.173-178
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• 2000

두 개의 페놀기를 포함하는 열린 고리형태의 1, 14-Bis(2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) 리간드를 염산염의 형태로 분리하여 원소 분석, 질량 스펙트럼 및 핵자기공명법으로 분석하였다. 합성된 리간드의 산 해리상수($logK^n{_H}$)와 $Cu^{2+}$, $Ni^{2+}$, $Co^{2+}$ 및 $Zn^{2+}$에 대한 안정도 상수($logK_{ML}$)를 전위차 적정법으로 결정하였다. 이때 온도는 $25^{\circ}C$ 및 이온강도는 0.10M($KNO_3$)로 고정시켰다. [Cu(bsated)] $(ClO_4)_2$ X-ray구조의 crystal data는 다음과 같다: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. tetrabutylammonium perchlorate 전해질의 dimethyl sulfoxide 용액속에서 [Cu(bsated)]$(ClO_4)_2$ 착물의 전기화학적 특성을 순환 전압-전류법 (CV)과 normal pulse voltammertry (NPV, 정상펄스전압전류법)으로 측정하였다.

• Bulletin of the Korean Chemical Society
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• 제33권9호
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• pp.2917-2924
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• 2012

Four novel metal-organic complexes $[Cd_2(IP)_2(TBZ)_2(H_2O)_2]{\cdot}(H_2O)$ (1), $[Zn_4(IP)_4(TBZ)_4]{\cdot}2(H_2O)$ (2), $[Zn_2(BTC)(TBZ)_2(CO_2H)]$ (3), [Co(PDC)(TBZ)] (4) (where IP = isophthalate; TBZ = thiabendazole; BTC = 1,3,5-benzenetricarboxylate; PDC = pyridine-3,4-dicarboxylate) have been prepared and characterized by IR spectrum, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. X-ray structure analysis reveals that 1, 2, and 3 are one-dimensional chain polymers, while 4 is a two-dimensional network polymer. The TBZ acts as a typical chelating ligand coordinated to the metal center in all complexes. The 1D chain architecture of 1 is constructed from isophthalates and cadmium atoms. A simultaneous presence of chelating, monodentate and bidentate coordination modes of IP ligands is observed in complex 2. In complex 3, the 16-membered rings are alternately arranged forming an infinite 1D double-chain structure. The 2D skeleton of 4 is formed by cobalt ions as nodes and PDC dianions as spacers, through coordination bonds. The hydrogen bonds and ${\pi}-{\pi}$ stacking play important roles in affecting the final structure where complexes 1 and 3 have 2D supramolecular networks, while complexes 2 and 4 have 3D supramolecular architectures.

• E2M - 전기 전자와 첨단 소재
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• 제8권6호
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• pp.780-786
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• 1995

For the execution of RIETAN program adopting Rietveld Analysis Method, the sample superconductor is made according to the solid state synthesis method at 920.deg. C for 24hrs, and was examined for the optimization of parameters needed to analyze Rietveld method with the input of the measured pattern data after measuring the pattern resulted from the X-ray diffraction. It was proven that the lattice constant of the superconductor which was consisted of Pmmm orthorhombic crystal structure in the analyzed space group correspond to the presented theoretical lattice constant a=3.8887(8).angs., b=3.8238(4).angs., c=11.7079.angs.. Therefore, it was examined and confin-ned that the R factor, which was compensated after analyzing the structure of superconductor resulted from this experimented data with the computer simulation, was refined to $R_{wp}$=8.83[%], $R_{P}$=6.47[%], $R_{I}$=10.08[%], $R_{F}$=7.19[%], $R_{E}$=3.76[%]. On the basis of these experimental data, the significant parameter such as the scale factor(S) and the zero point shift(Z) and FWHM value(U,V,W) were optimized as follows; S=2.0827E-3, Z=0.2146, U=4.2761E-2, V=1.7983E-2, and W=2.6768E-2.2.2.2.2.2.

• 한국세라믹학회지
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• 제49권3호
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• pp.205-215
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• 2012

It has been studied the crystal and block structures of the hexagonal ferrites with M, W, Y and Z types prepared by various coprecipitation-oxidation method. The structures have been refined with a Rietveld analysis of the powder X-ray diffraction pattern with high precision ($R_{WP}$ <0.09, $R_I$ <0.03). The density difference between the S-blocks was proportioned to the cobalt contents in hexagonal ferrites, but that between the R or T-blocks was relatively small. Compared with the blocks and cation-oxygen polyhedra in BaM ($BaFe_{12}O_{19}$), those were bulky to the normal direction for the c-axis in $Co_2W$ ($BaCo_2Fe_{16}O_{27}$) and to the parallel direction for the c-axis in $Co_2Y$ ($Ba_2Co_2Fe_{12}O_{22}$) and $Co_2Z$ ($Ba_3Co_2Fe_{24}O_{41}$). The S-blocks of $Co_2W$, $Co_2Y$, and $Co_2Z$ were unstable and distorted. Because the T-block of $Co_2Z$ was unstable, the T-block was decomposed into the Ba-rich phase and $Co_2W$ at high temperatures above $1200^{\circ}C$. A standard powder X-ray diffraction pattern for $Co_2Z$ was proposed as well.

• 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.

• Carbon letters
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• 제14권2호
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• pp.94-98
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• 2013

Isotropic pitch fibers were stabilized and carbonized for preparing carbon fibers. To optimize the duration and temperature during the stabilization process, a thermogravimetric analysis was conducted. Stabilized fibers were carbonized at 1000, 1500, and $2000^{\circ}C$ in a furnace under a nitrogen atmosphere. An elemental analysis confirmed that the carbon content increased with an increase in the carbonization temperature. Although short graphitic-like layers were observed with carbon fibers heat-treated at 1500 and $2000^{\circ}C$, Raman spectroscopy and X-ray diffraction revealed no significant effect of the carbonization temperature on the crystalline structure of the carbon fibers, indicating the limit of developing an ordered structure of isotropic pitch-based carbon fibers. The electrical conductivity of the carbonized fiber reached $3.9{\times}10^4$ S/m with the carbonization temperature increasing to $2000^{\circ}C$ using a four-point method.

• Bulletin of the Korean Chemical Society
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• 제33권6호
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• pp.1929-1933
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• 2012

Two cobalt(II) compounds $[Co(2,2{^\prime}-bipy)(H_2O)_2(SO_4)]_n$ (1) and $[Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6]{\cdot}2H_2O$ (2) (2,2'-bipy = 2,2'-bipyridine, $H_4btec$ = 1,2,4,5-benzenetetracarboxylic acid), have been simultaneously synthesized by a one-pot slow solvent evaporation reaction. Their structures were determined by single-crystal X-ray diffraction and further characterized by X-ray powder diffraction (XRPD), IR, elemental and thermogravimetric analysis (TGA). The structural analysis reveals that compound 1 exhibits an infinite 1D chain structure with the octahedral Co(II) centers bridging by the tetrahedral ${\mu}_2-SO{_4}^{2-}$ ligands, while compound 2 possesses a dinuclear $Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6$ unit and the two adjacent octahedral Co(II) ions are linked by the bismonodentately coordinated btec ligand. Additionally, compound 2 exhibits blue fluorescent emission in the solid state at room temperature.