• Title/Summary/Keyword: X-ray Structure Analysis

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Synthesis of Novel Platinum Precursor and Its Application to Metal Organic Chemical Vapor Deposition of Platinum Thin Films

  • Lee, Sun-Sook;Lee, Ho-Min;Park, Min-Jung;An, Ki-Seok;Kim, Jin-Kwon;Lee, Jong-Heun;Chung, Taek-Mo;Kim, Chang-Gyoun
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1491-1494
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    • 2008
  • A novel platinum aminoalkoxide complex, Pt$(dmamp)_2$ has been prepared by the reaction of cis-$(py)_2PtI_2$ with two equivalents of Na(dmamp) (dmamp = 1-dimethylamino-2-methyl-2-propanolate). Single-crystal X-ray crystallographic analysis shows that the Pt(dmamp)2 complex keeps a square planar geometry with each two nitrogen atoms and two oxygen atoms having trans configuration. Platinum films have been deposited on TaN/ Ta/Si substrates by metal organic chemical vapor deposition (MOCVD) using Pt$(dmamp)_2$. As-deposited platinum thin films did not contain any appreciable amounts of impurities except a little carbon. As the deposition temperature was increased, the films resistivity and deposition rate increased. The electrical resistivity (13.6 $\mu\Omega$cm) of Pt film deposited at 400 ${^{\circ}C}$ is a little higher than the bulk value (10.5 $\mu\Omega$cm) at 293 K. The chemical composition, crystalline structure, and morphology of the deposited films were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, and atomic force microscopy.

Analysis of Reflectivity for Interfacial Roughness of Depth-Graded W/Si Multilayer Mirror (두께 변화 W/Si 다층박막거울의 계면 거칠기에 대한 반사율 분석)

  • Chon, Kwon Su
    • Journal of the Korean Society of Radiology
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    • v.12 no.1
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    • pp.101-106
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    • 2018
  • Multilayer mirrors have widely been used for monochromatization of X-ray with high reflection efficiency. The reflected X-ray energy or wavelength is determined by the d-spacing of a multilayer mirror and the incidence angle. The reflectivity critically depends on the number of bilayers and surface roughness on each interface. The multilayer mirror has a structure of alternative deposition of high and low Z-elements on the substrate. Each interface should be considered in the calculation of reflectivity. In this paper, we examine the degradation of reflectivity by the inter-diffusion combined with surface roughness on each interface for a W/Si multilayer mirror. In the depth-graded W/Si multilayer mirror, the FWHMs for angle and energy were larger than them of the uniform multilayer mirror. Inter-diffusion considerable gave rise to the degradation of reflectivity. To obtain measured reflectivity closed to the expected reflectivity, the inter-diffusion on W-Si and Si-W interfaces should be considered.

Variations in electrode characteristics through simplification of phosphorus-doped NiCo2O4 electrode manufacturing process (인이 도핑된 NiCo2O4 전극 제조 공정의 간소화를 통한 전극 특성의 변화)

  • Seokhee-Lee;Hyunjin Cha;Jeonghwan Park;Young Guk Son;Donghyun Hwang
    • Journal of the Korean institute of surface engineering
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    • v.56 no.5
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    • pp.299-308
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    • 2023
  • In this study, phosphorus (P)-doped nickel cobaltite (P-NiCo2O4) and nickel-cobalt layered double hydroxide (P-NiCo-LDH) were synthesized on nickel (Ni) foam as a conductive support using hydrothermal synthesis. The thermal properties, crystal structure, microscopic surface morphology, chemical distribution, electronic state of the constituent elements on the sample surface, and electrical properties of the synthesized P-NiCo2O4 and P-NiCo-LDH samples were analyzed using thermogravimetric analysis-differential scanning calorimetry (TGA-DSC), X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). The P-NiCo2O4 electrode exhibited a specific capacitance of 1,129 Fg-1 at a current density of 1 Ag-1, while the P-NiCo-LDH electrode displayed a specific capacitance of 1,012 Fg-1 at a current density of 1 Ag-1. When assessing capacity changes for 3,000 cycles, the P-NiCo2O4 electrode exhibited a capacity retention rate of 54%, whereas the P-NiCo-LDH electrode showed a capacity retention rate of 57%.

Promoting Effect of MgO in the Photodegradation of Methylene Blue Over MgO/MWCNT/TiO2 Photocatalyst

  • Chen, Ming-Liang;Zhang, Feng-Jun;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.20 no.7
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    • pp.345-350
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    • 2010
  • For the present paper, we prepared MgO/MWCNT/$TiO_2$ photocatalyst by using multi-walled carbon nanotubes (MWCNTs) pre-oxidized by m-chlorperbenzoic acid (MCPBA) with magnesium acetate tetrahydrate $(Mg(CH_2COO)_2\cdot4H_2O)$ and titanium n-butoxide $(Ti\{OC(CH_3)_3\}_4)$ as magnesium and titanium precursors. The prepared photocatalyst was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. The decomposition of methylene blue (MB) solution was determined under irradiation of ultraviolet (UV) light. The XRD results show that the MgO/MWCNT/$TiO_2$ photocatalyst have cubic MgO structure and anatase $TiO_2$ structure. The porous structure and the $TiO_2$ agglomerate coated on the MgO/MWCNT composite can be observed in SEM images. The Mg, O, Ti and C elements can be also observed in MgO/MWCNT/$TiO_2$ photocatalyst from EDX results. The results of photodegradation of MB solution under UV light show that the concentration of MB solution decreased with an increase of UV irradiation time for all of the samples. Also, the MgO/MWCNT/$TiO_2$ photocatalyst has the best photocatalytic activity among these samples. It can be considered that the MgO/MWCNT/$TiO_2$ photocatalyst had a combined effect, the effect of MWCNT, which could absorb UV light to create photoinduced electrons $(e^-)$, and the electron trapping effect of MgO, which resulted in an increase of the photocatalytic activity of $TiO_2$.

Mapping the Mass of the Double Radio Relic Merging Galaxy Cluster PLCK G287+32.9: A Subaru and HST Weak-lensing Analysis

  • Finner, Kyle;Jee, Myungkook James;Dawson, William;Golovich, Nathan;Gruen, Daniel;Lemaux, Brian;Wittman, David
    • The Bulletin of The Korean Astronomical Society
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    • v.42 no.2
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    • pp.41.2-41.2
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    • 2017
  • Discovered as the second highest S/N detection of the Planck SZ survey, PLCK G287.0+32.9 is a massive galaxy cluster that belongs to a rare collection of merging clusters that exhibit two radio relics and a radio halo. A feature that makes this cluster even more unique is the separation of the radio relics with one $\sim 400$ kpc to the north-west of the X-ray peak and the other $\sim 2.8$ Mpc to the south-east. This asymmetric configuration requires a complex merging scenario. A key to gaining insight into the events that caused the formation of the merging features is to understand the dark matter mass distribution. Using a weak-lensing technique on deep Subaru and Hubble Space Telescope observations, we map the dark matter mass distribution of PLCK G287.0+32.9. Our investigation detects five significant mass structures. The mass is dominated by a primary structure that is centered near the X-ray peak of the intracluster medium. Four lesser mass structures are detected with two located within $\sim 1\arcmin$ of the primary mass structure, a third to the north-west, and a fourth near the south-east radio relic. Along with these detections, we estimate the mass of each structure and relate their distributions to the intracluster medium and galaxy distributions. In addition, we discuss the relation of the mass structures to the formation of the relics and plausible merging scenarios.

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Two New closo- or nido-Carborane Diphosphine Complexes: Synthesis, Characterization and Crystal Structures

  • Kong, Lingqian;Zhang, Daopeng;Su, Fangfang;Li, Dacheng;Dou, Jianmin
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2249-2252
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    • 2011
  • Two new carborane complexes containing closo- or nido-carborane diphosphine ligands with the formula: complex $[Hg(7,8-(PPh_2)_2-7,8-C_2B_9H_{10})_2]$ $CH_2Cl_2$ (1) and $[Ag_2({\mu}-Cl)_2(1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10})_2]$ (2) have been synthesized and characterized by elemental analysis, 1H and 13C NMR spectroscopy and X-ray structure determination. The X-ray structure analyses revealed that the carborane diphosphine ligand was degraded from closo-1,2-$(PPh_2)_2-1,2-C_2B_{10}H_{10}$ to nido-[$7,8-(PPh_2)_2-7,8-C_2B_9H_{10}]^-$ in complex 1, while the closo nature of the starting ligand $1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10}$ was retained in complex 2. In either of the two complexes, the carborane diphosphine ligand was coordinated bidentately to the Hg(II) or Ag(I) center through its two phosphorus atoms, therefore forming a five-member cheating ring between the carborane ligand and the metal center. The coordination geometry of the metal atom is distorted tetrahedron formed by $P_4$ unit in complex 1 and $P_2Cl_2$ unit in complex 2, respectively.

Crystallographic analysis of dehydrated fully Tl+-exchanged zeolite Y

  • Lim, Woo Taik;Kwon, Ji Hye;Choi, Sik Young;Kim, Young Hun;Heo, Nam Ho
    • Analytical Science and Technology
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    • v.18 no.4
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    • pp.278-286
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    • 2005
  • The crystal structure of ($Tl_{71}$-Y ($Tl_{71}Si_{121}Al_{71}O_{384}$), ${\alpha}=24.706(3){\AA}$, dehydrated at 653 K and $8{\times}10^{-6}$ torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group $Fd\bar{3}m$ at 294(1) K. The structure was refined using all intensities to the final error indices (using only the 302 reflection for which $F_{\circ}$ > $4{\sigma}(F_0)$) $R_1=0.0602$ (based on F) and $R_w=0.1744$ (based on $F_2$). The 71 $Tl^+$ ions per unit cell are found at four crystallographically distinct positions. Site I' position in the sodalite cavity opposite D6Rs are each occupied by eighteen $Tl^+$ ions per unit cell; these $Tl^+$ ions are recessed ca. $1.45{\AA}$ into the sodalite cavity from their O(3) plane (Tl-O=2.701(15), $3.163(16){\AA}$ and O-Tl-O=$92.1(4)^{\circ}$). The 23 $T1^+$ ions fill site II in the supercage; these $T1^+$ ions are recessed ca. $1.58{\AA}$ into the supercage from their O(2) plane (Tl-O = 2.850(16), $3.156(16){\AA}$ and O-T1-O = $85.1(5)^{\circ}$). The 19 $Tl^+$ ions lie at site III' in the supercage near a triple 4-ring (Tl-O = 3.10(7), $3.39(5){\AA}$ and O-Tl-O = 47.8(9), $95.3(18)^{\circ}$) and the remaining II ions occupy another site III' near a triple 4-ring in the supercage (Tl-O = 2.81(4), $2.71(4){\AA}$ and O-Tl-O = $57.3(8)^{\circ}$).

MWCNT, silver nanoparticles, CuBTC를 사용한 염소 이온 센서 합성

  • Gwak, Byeong-Gwan;Park, Su-Bin;Yu, Bong-Yeong
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.101-101
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    • 2018
  • Quantitative measurement of chloride ion concentration has an important role in various fields of electrochemistry, medical science, biology, metallurgy, architecture, etc. Among them, its importance of architecture is ever-growing due to unexpected degradations of building structure. These situations are caused by corrosion of reinforced concrete (RC) structure of buildings. And chloride ions are the most powerful factors of RC structure corrosion. Therefore, precise inspection of chloride ion concentration must be required to increase the accuracy of durability monitoring. Multi-walled Carbon nanotubes (MWCNTs) have high chemical resistivity, large surface area and superior electrical property. Thus, it is suitable for the channels of electrical signals made by the sensor. Silver nanoparticles were added to giving the sensing property. CuBTC, one of the metal organic frameworks (MOFs), was employed as a material to improve the sensing property because of its hydrophilicity and high surface area to volume ratio. In this study, sensing element was synthesized by various chemical reaction procedures. At first, MWCNTs were functionalized with a mixture of sulfuric acid and nitric acid because of enhancement of solubility in solution and surface activation. And functionalized MWCNTs, silver nanoparticles, and CuBTC were synthesized on PTFE membrane, one by one. Electroless deposition process was performed to deposit the silver nanoparticles. CuBTC was produced by room temperature synthesis. Surface morphology and composition analysis were characterized by scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS), respectively. X-ray photoelectron spectroscopy (XPS) was also performed to confirm the existence of sensing materials. The electrical properties of sensor were measured by semiconductor analyzer. The chloride ion sensing characteristics were confirmed with the variation of the resistance at 1 V.

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Fabrication of CuO/ZnO Nano-heterostructure by Photochemical Method and Their H2S Gas Sensing Properties

  • Kim, Jae-Hyun;Yong, Ki-Jung
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.359-359
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    • 2011
  • This study reports the H2S gas sensing properties of CuO / ZnO nano-hetero structure bundle and the investigation of gas sensing mechanism. The 1-Dimensional ZnO nano-structure was synthesized by hydrothermal method and CuO / ZnO nano-heterostructures were prepared by photo chemical reaction. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) spectra confirmed a well-crystalline ZnO of hexagonal structure. In order to improve the H2S gas sensing properties, simple type of gas sensor was fabricated with ZnO nano-heterostructures, which were prepared by photo-chemical deposition of CuO on the ZnO nanorods bundle. The furnace type gas sensing system was used to characterize sensing properties with diluted H2S gas (50 ppm) balanced air at various operating temperature up to 500$^{\circ}C$. The H2S gas response of ZnO nanorods bundle sensor increased with increasing temperature, which is thought to be due to chemical reaction of nanorods with gas molecules. Through analysis of X-ray photoelectron spectroscopy (XPS), the sensing mechanism of ZnO nanorods bundle sensor was explained by well-known surface reaction between ZnO surface atoms and hydrogen sulfide. However at high sensing temperature, chemical conversion of ZnO nanorods becomes a dominant sensing mechanism in current system. Photo-chemically fabricated CuO/ZnO heteronanostructures show higher gas response and higher current level than ZnO nanorods bundle. The gas sensing mechanism of the heteronanostructure can be explained by the chemical conversion of sensing material through the reaction with H2S gas.

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Preparation and Cyclic Performance of Li1.2(Fe0.16Mn0.32Ni0.32)O2 Layered Cathode Material by the Mixed Hydroxide Method

  • Karthikeyan, K.;Nam, K.W.;Hu, E.Y.;Yang, X.Q.;Lee, Y.S.
    • Bulletin of the Korean Chemical Society
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    • v.34 no.7
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    • pp.1995-2000
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    • 2013
  • Layered $Li_{1.2}(Fe_{0.16}Mn_{0.32}Ni_{0.32})O_2$ was prepared by the mixed hydroxide method at various temperatures. Xray diffraction (XRD) pattern shows that this material has a ${\alpha}-NaFeO_2$ layered structure with $R{\bar{3}}m$ space group and that cation mixing is reduced with increasing synthesis temperature. Scanning electron microscopy (SEM) reveals that nano-sized $Li_{1.2}(Fe_{0.16}Mn_{0.32}Ni_{0.32})O_2$ powder has uniform particle size distribution. X-ray absorption near edge structure (XANES) analysis is used to study the local electronic structure changes around the Mn, Fe, and Ni atoms in this material. The sample prepared at $700^{\circ}C$ delivers the highest discharge capacity of 207 $mAhg^{-1}$ between 2-4.5 V at 0.1 $mAcm^{-2}$ with good capacity retention of 80% after 20 cycles.