• Title/Summary/Keyword: X-ray diffraction analysis(XRD)

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Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

Crystallographical Characteristics of Solar Salts Produced from Jeonnam Area by X-Ray Diffraction Technique (X선 회절법에 의한 전남지역 천일염의 결정학적 특성)

  • Jeong, Byung-Jo;Kim, Yong;Kim, Chang-Dae;Hyun, Seung-Cheol;Ham, Gyung-Sik
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.9
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    • pp.1284-1288
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    • 2009
  • Identification of various inorganic compound crystals contained in solar salts, which are produced from 12 areas of Jeonnam, was firstly made by the X-ray diffraction (XRD) technique. The analysis of the XRD spectra was carried out on the basis of Joint Committee on Powder Diffraction Standards (JCPDS) data and the results of Energy Dispersive X-ray Spectrometer (EDX) measurements. In particular, the analysis of the XRD spectra supported that each solar salt contains $Na_2S$ (Shinan Jeungdo and Sinui), $KMgCl_3$ (Shinan Bigeum), $Ca(ClO_3)_2$ (Shinan Docho), $CaAl_4O_7$ (Haenam Songji), $CaSiO_3$ and $CaCl_2$ (Goheung) as inorganic compound crystals, which have not been reported for the solar salts. Also, the XRD results indicated that the solar salts maintain a cubic NaCl crystal structure without any change of lattice parameters etc. However, it was shown in the Field Emission Scanning Electron Microscope (FE-SEM) images that an external form of the solar salts has a lamination layer shape of a cubic structure, which is different from a simple cubic form for the purified salts and the reagent NaCl.

Effects of Oxide Layer Formed on TiN Coated Silicon Wafer on the Friction and Wear Characteristics in Sliding (미끄럼운동 시 TiN 코팅에 형성되는 산화막이 마찰 및 마멸 특성에 미치는 영향)

  • 조정우;이영제
    • Tribology and Lubricants
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    • v.18 no.4
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    • pp.260-266
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    • 2002
  • In this study, the effects of oxide layer farmed on the wear tracks of TiN coated silicon wafer on friction and wear characteristics were investigated. Silicon wafer was used for the substrate of coated disk specimens, which were prepared by depositing TiN coating with 1 ${\mu}{\textrm}{m}$ in coating thickness. AISI 52100 steel ball was used fur the counterpart. The tests were performed both in air for forming oxide layer on the wear track and in nitrogen to avoid oxidation. This paper reports characterization of the oxide layer effects on friction and wear characteristics using X-ray diffraction(XRD), Auger electron spectroscopy(AES), scanning electron microscopy (SEM) and multi-mode atomic force microscope(AFM).

미끄럼운동 시 TiN코팅에 형성되는 산화막이 마찰 및 마멸 특성에 미치는 영향

  • Jo, Jeong-U;Im, Jeong-Sun;U, Sang-Gyu;Lee, Yeong-Je
    • Proceedings of the Korean Society of Tribologists and Lubrication Engineers Conference
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    • 2002.05a
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    • pp.310-316
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    • 2002
  • In this study, the effects of oxide layer formed on the wear tracks of TiN coated silicon wafer on friction and wear characteristics were investigated. Silicon wafer was used for the substrate of coated disk specimens, which were prepared by depositing TiN coating with $1{\mu}m$ in coating thickness. AISI 52100 steel ball was used for the counterpart. The tests were performed both in air for forming oxide layer on the wear track and in nitrogen to avoid oxidation. This paper reports characterization of the oxide layer effects on friction and wear characteristics using X-ray diffraction (XRD). Auger electron spectroscopy (AES), scanning electron microscopy (SEM) and sliding tests.

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Characterization of vanadium carbide coating deposited by borax salt bath process

  • Aghaie-Khafri, M.;Daemi, N.
    • Advances in materials Research
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    • v.1 no.3
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    • pp.233-243
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    • 2012
  • Thermal reactive diffusion coating of vanadium carbide on DIN 2714 steel substrate was performed in a molten borax bath at $950-1050^{\circ}C$. The coating formed on the surface of the substrate had uniform thickness ($1-12{\mu}m$) all over the surface and the coating layer was hard (2430-2700 HV), dense, smooth and compact. The influence of the kinetics parameters, temperature and time, has been investigated. Vanadium carbide coating was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX) and X-ray diffraction analysis (XRD). The corrosion resistance of the coating was evaluated by potentiodynamic polarization in 3.5% NaCl solution. The results obtained showed that decrease of coating microhardness following increasing time and temperature is owing to the coarsening of carbides and coating grain size.

A Basic Study on the Refractory Material of Kalcheon Iron Making Furnace (갈천리 야철로 내화재료의 기초적 연구)

  • HAN, S. M.;KIM, K. N.;SHIN, D. Y.
    • Journal of Conservation Science
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    • v.2 no.2 s.2
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    • pp.25-30
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    • 1993
  • Materials (refractory, stone) of iron making furnace excavated from Kalcheon were investigated by the scanning electron microscopy(SEM) with an energy dispersive X-ray analysis (EDAX), X-ray fluorescence(XRF), and X-ray diffraction(XRD). Chemical composition of the refractory materials were $SiO_2(68.74\%),\;Al_2O_3(18.40\%),\;CaO(0.42\%),\;MgO(1.04\%)\;and\;K_2O(2.26\%)$ in weight ratio, which were the typical components presented in common clay. The results of chemical analysis for the stone and the glaze coated, alkali ion(K, Na, Ca) components of the glaze contained high concentration than that the stone. It was suggested that this change had a close relationship with the kinds of fuels used.

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Stage transformation characteristice of Li, K and Na-graphite intercalation compounds (Li, K과 Na-흑연 층간화합물의 stage 전이특성)

  • 오원춘;임창성;오근호;고영신
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.1
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    • pp.83-90
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    • 1998
  • Stage transformation characteristics of Li, K and Na-graphite deintercalation compounds (GDICs) were studied under consideration of a deintercalation mechanism of the intercalants between carbon layers. Li-graphite intercalation compounds (GICs) synthesized by a controlling temperatures and pressures have been spontaneously decomposed in the atmosphere. By X-ray differaction analysis the $d_{001}$-values of stage 1 and 2 were identified to be 3.71 and 7.06 $\AA$, respectively. After 6 weeks, the deintercalation reaction of the Li-GICs ceased and only residual compounds could be observed. K-GICs were synthesized by the modified two-bulb method resulting in structural stabilities and stage transitions. By X-ray diffraction analysis the very stable K-graphite residue compounds were observed after 10 weeks. Na-GICs with stage 1 and 2 were synthesized using the high temperature and pressure technique. The temperature dependence of a deintercalation reaction and a thermal stability of Na-GICs were discussed. The structure changes of the Na-GDICs depending on heating rates were identified by X-ray diffraction. According to the deintercalation process, the stage transformations could be attributed to irregular deintercalations of the GDICs with disordered stage.

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Preparation and Characterization of Crystalline Carbon Nitride (결정질 질화탄소 박막의 합성과 그 특성 해석)

  • 김종일;배선기
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.10
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    • pp.835-844
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    • 2001
  • In this paper, we report the successful growth of crystalline carbon nitride films in Si(100) by a laser-electric discharge method. The laser ablation of the target leads to vapor plume plasma expending into the ambient nitrogen arc discharge area. X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy(AES) were used to identify the binding structure and the content of the nitrogen species in the deposited films. The surface morphology of the films with a deposition time of 2 hours is studied using a scanning electron microscopy (SEM). In order to determine the structural crystalline parameters, X-ray diffraction (XRD) was used to analysis the grown films.

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Synthesis and Characterization of Metal (Pt, Pd and Fe)-graphene Composites

  • Chen, Ming-Liang;Park, Chong-Yeon;Choi, Jong-Geun;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.48 no.2
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    • pp.147-151
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    • 2011
  • In this study, we prepared graphene by using the modified Hummers-Offeman method and then introduced the metals (Pt, Pd and Fe) for dispersion on the surface of the graphene for synthesis of metal-graphene composites. The characterization of the prepared graphene and metal-graphene composites was performed by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis and transmission electron microscopy (TEM). According to the results, it can be observed that the prepared graphene consists of thin stacked flakes of shapes having a well-defined multilayered structure at the edge. And the metal particles are dispersed uniformly on the surface of the graphene with an average particle size of 20 nm.

Effect of Annealing on Carbon Nitride Films Prepared by High Voltage Discharge Plasma (고전압 방전 플라즈마에 의해 합성한 질화탄소 박막의 열처리 효과)

  • 김종일
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.15 no.5
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    • pp.455-459
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    • 2002
  • I have investigated the effects of annealing on a polymeric $\alpha-C_3N_{4.2}$ at high pressure and temperature in the presence of seeds of crystalline carbon nitride films prepared by a high voltage discharge plasma. The samples were evaluated by x-ray photoelectron spectroscopy (XPS), infrared spectroscopy, Auger electron spectroscopy and x-ray diffraction(XRD). Notably, XPS studies of the film composition before and after annealing demonstrate that the nitrogen composition in $\alpha-C_3N_{4.2}$ material initially containing more than 58% nitrogen decreases during the annealing process and reaches a common, stable composition of ~43%. XPS analysis also shows that the nitrogen composition in the annealed films without polymeric $\alpha-C_3N_{4.2}$ was reduced from 35% to 17%. Furthermore the concentration of the sp$^3$bonded phase increased with the increment of the annealing temperature.