• 제목/요약/키워드: X-ray microscopy

검색결과 3,210건 처리시간 0.025초

비결정질 코발트 인산염 합성 및 NaBH4 가수분해를 통한 수소발생 촉매 활성 연구 (Synthesis of Cobalt Phosphates and their Catalytic Properties of the Hydrogen Generation from the Hydrolysis of NaBH4)

  • 김영용;박준범;권기영
    • 공업화학
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    • 제26권6호
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    • pp.743-745
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    • 2015
  • 본 연구에서는 실온에서 간단히 염기의 양을 조절함으로서 세 가지 종류의 서로 다른 형태의 비결정질의 cobalt phosphate를 합성하였다. 합성된 샘플의 결정성과 형태를 X-Ray Diffraction (XRD)과, Scanning Electron Microscopy (SEM)를 통하여 확인하였으며, sodium borohydride의 수소발생 불균일 촉매로서 적용하였다. 촉매들 중에서 실온에서 합성한 비결정질의 cobalt phosphate 중에서 염기의 양이 가장 적은 10 nm 이하의 얇은 판상 형태의 촉매가 표면적이 넓어 가장 좋은 수소 발생 촉매활성을 보였다.

Synthesis of Praseodymium-Doped TiO2 Nanocatalysts by Sol-Microwave and Their Photocatalytic Activity Study

  • Huang, Fengping;Wang, Shuai;Zhang, Shuang;Fan, Yingge;Li, Chunxue;Wang, Chuang;Liu, Chun
    • Bulletin of the Korean Chemical Society
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    • 제35권8호
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    • pp.2512-2518
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    • 2014
  • The praseodymium-doped $TiO_2$ photocatalyst samples, which could degrade methyl orange under UV irradiation, were prepared by sol-microwave method for improving the photocatalytic activity of $TiO_2$. The resulting materials were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman spectra, Fourier transform infrared spectra (FTIR) and Ultraviolet-visible diffuse reflectance spectra (UV-vis DRS). It was found Pr doping retarded the growth of crystalline size and the phase transformation from anatase to rutile, and narrowed the band gap energy. Praseodymium doping brought about remarkable improvement in the photoactivity. The optimal dopant amount of Pr was 2% by molar of cement and the calcination temperature was $500^{\circ}C$ for the best photocatalytic activity. The improvement of photocatalytic activity was ascribed to the occurrence of lattice distortion and the effective containment of the recombination of the electron-hole by $Pr^{3+}$.

전자회절실험에 의한 알루미늄 합금 (Al-Cu-Mg)의 미세 S-상 석출입자에 대한 결정구조 연구 (A Study of the Crystal Structure of the Fine S-Phase Precipitate in Al-Cu-Mg Alloy by Electron Diffraction Experiments)

  • 김황수
    • Applied Microscopy
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    • 제35권4호
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    • pp.1-9
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    • 2005
  • 이 논문에서 Al-Cu-Mg 합금의 미세 석출 입자의 S-상 ($Al_2CuMg$) 결정구조에 대해 전자회절실험에 의한 포괄적인 연구 결과가 보고 되어 있다. 이 실험에는 한 S-상 입자를 포함하는 최소 영역의 일정 zone축의 회절패턴(SAED) 관찰과 이에 대응되는 운동학적 이론을 기초로 한 패턴의 시물레이션과의 비교 분석, 그리고 관측된 회절 패턴 필름으로부터 각 Bragg회절 점의 강도의 정량적 데이터 추출과 운동학적 및 동역학적 회절 강도 계산과의 비교 검토의 과정을 포함하고 있다. 이러한 연구의 한 결과 S-상의 결정구조는 일찍이 X-ray 방법으로부터 얻은 PW 모델결정(Perlitz and Westgren, 1943)과 일치함을 보여주고 있고, HREM 방법에 의해 새로이 구한 RaVel (Radmilovic et al., 1999) 모델과는 전혀 맞지않음이 판명되었다.

Fabrication of ZnO Nanostructures with Various Growth Conditions by Vapor Phase Transport

  • Kim, So-A-Ram;Nam, Gi-Woong;Kim, Min-Su;Yim, Kwang-Gug;Kim, Do-Yeob; Leem, Jae-Youn
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2011년도 제41회 하계 정기 학술대회 초록집
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    • pp.250-250
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    • 2011
  • Zinc oxide (ZnO) structures have great potential in many applications. Currently, the most commonly used method to grow ZnO nanostructres are the vapor transport method (VPT). The morphology of the ZnO structures largely related to the growth conditions, including growth temperature, distance between the substrate and source, and gas ambient. Previously ZnO nanosturecutres with high crystallinity were obtained at the growth temperature of 800$^{\circ}C$, in the argon and oxygen gas ambient. In this study, we report the properties of the ZnO nanostructures, which were synthesized on Au-catalyzed Si substrate by VPT, using a mixture of ZnO and graphite powders as source material under the different condition, including gas ratio of argon/oxygen and distance between substrate and source at the growth temperature of 800$^{\circ}C$. The structural and optical properties of the ZnO nanostructures were investigated by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and photoluminescence (PL).

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Pt Electrocatalysts Composited on Electro-Spun Pt Nanowires for Direct Methanol Fuel Cells

  • An, Geon-Hyoung;Ahn, Hyo-Jin
    • 한국재료학회지
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    • 제22권8호
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    • pp.421-425
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    • 2012
  • Two types of Pt nanoparticle electrocatalysts were composited on Pt nanowires by a combination of an electrospinning method and an impregnation method with NaBH4 as a reducing agent. The structural properties and electrocatalytic activities for methanol electro-oxidation in direct methanol fuel cells were investigated by means of scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry. In particular, SEM, HRTEM, XRD, and XPS results indicate that the metallic Pt nanoparticles with polycrystalline property are uniformly decorated on the electro-spun Pt nanowires. In order to investigate the catalytic activity of the Pt nanoparticles decorated on the electro-spun Pt nanowires, two types of 20 wt% Pt nanoparticles and 40 wt% Pt nanoparticles decorated on the electro-spun Pt nanowires were fabricated. In addition, for comparison, single Pt nanowires were fabricated via an electrospinning method without an impregnation method. As a result, the cyclic voltammetry and chronoamperometry results demonstrate that the electrode containing 40 wt% Pt nanoparticles exhibits the best catalytic activity for methanol electro-oxidation and the highest electrochemical stability among the single Pt nanowires, the 20 wt% Pt nanoparticles decorated with Pt nanowires, and the 40 wt% Pt nanoparticles decorated with Pt nanowires studied for use in direct methanol fuel cells.

$Ni_3$Al의 기계적합금화에 미치는 $Y_2O_3$ 첨가의 영향 (The Effect of $Y_2O_3$ Addition on the Mechanical Alloying of $Ni_3$Al)

  • 이상태
    • 한국분말재료학회지
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    • 제4권3호
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    • pp.205-213
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    • 1997
  • Mechanical alloying of $Ni_3Al$ and $Y_2O_3$ added ODS $Ni_3Al$ from elemental powders was investigated by the X-ray diffraction, differential scanning calorimeter, transmission electron microscopy and optical microscopy. The steady states of $Ni_3Al$ and ODS $Ni_3Al$ powders were reached after mechanical alloying with the condition of the ball-to-powder input ratio of 20:1 for 20 hours and 10 hours, respectively. The addition of nano-sized $Y_2O_3$ particles enhanced cold working and fracture, and subsequently accelerated MA of $Ni_3Al$ powders. DSC results of MAed $Ni_3Al$ powders showed four exothermic peaks at 14$0^{\circ}C$, 234$^{\circ}C$, 337$^{\circ}C$ and 385$^{\circ}C$. From the high temperature X-ray diffraction analysis, it was concluded that the peaks were resulted from the recovery solution of unalloyed Al in Ni, the formation of intermediate phase NiAl, and $LI_2$ ordering of MAed $Ni_3Al$ powders.

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Synthesis and Characterization of ZnS and ZnS/TiO2 Nanocomposites and Their Enhanced Photo-decolorization of MB and 1,5-Diphenyl Carbazide

  • Meng, Ze-Da;Ullah, Kefayat;Zhu, Lei;Ye, Shu;Oh, Won-Chun
    • 한국세라믹학회지
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    • 제51권4호
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    • pp.307-311
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    • 2014
  • ZnS and $ZnS/TiO_2$ were prepared by chemical deposition. The prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and transmission electron microscopy (TEM). The generation of reactive oxygen species was detected by monitoring the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). Excellent catalytic degradation of methylene blue (MB) solution was observed using the $ZnS/TiO_2$ composites during irradiation with visible light. The results show that the photocatalytic performance of $TiO_2$ nanoparticles is improved by loading with ZnS.

Preparation of ZnO2 Nanoparticles Using Organometallic Zinc(II) Isobutylcarbamate in Organic Solvent

  • Kim, Kyung-A;Cha, Jae-Ryung;Gong, Myoung-Seon;Kim, Jong-Gyu
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.431-435
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    • 2014
  • Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

Heteroepitaxial Growth of Single 3C-SiC Thin Films on Si (100) Substrates Using a Single-Source Precursor of Hexamethyldisilane by APCVD

  • Chung, Gwiy-Sang;Kim, Kang-San
    • Bulletin of the Korean Chemical Society
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    • 제28권4호
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    • pp.533-537
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    • 2007
  • This paper describes the heteroepitaxial growth of single-crystalline 3C-SiC (cubic silicon carbide) thin films on Si (100) wafers by atmospheric pressure chemical vapor deposition (APCVD) at 1350 oC for micro/nanoelectromechanical system (M/NEMS) applications, in which hexamethyldisilane (HMDS, Si2(CH3)6) was used as a safe organosilane single-source precursor. The HMDS flow rate was 0.5 sccm and the H2 carrier gas flow rate was 2.5 slm. The HMDS flow rate was important in obtaing a mirror-like crystalline surface. The growth rate of the 3C-SiC film in this work was 4.3 μm/h. A 3C-SiC epitaxial film grown on the Si (100) substrate was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), reflection high energy electron diffraction (RHEED), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Raman scattering, respectively. These results show that the main chemical components of the grown film were single-crystalline 3C-SiC layers. The 3C-SiC film had a very good crystal quality without twins, defects or dislocations, and a very low residual stress.

Crystal growth and characteristics of lysozyme crystals

  • Kojima, Kenichi
    • 한국결정학회:학술대회논문집
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    • 한국결정학회 2002년도 정기총회 및 추계학술연구발표회
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    • pp.3-3
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    • 2002
  • Many studies on crystal growth mechanisms of the hen egg-white lysozyme protein crystals have mainly performed by optical microscopy and atomic force microscopy (AFM). As results, two types of growth mechanisms, which are a two-dimensional nucleation mechanism and a spiral growth mechanism, were identified. However, there was no direct evidence of grown-in screw dislocations at the spiral sites. We first observed the screw dislocations in tetragonal lysozyme crystals using synchrotron X-ray topography. In addition, to confirm the characteristics of dislocations, we have observed some elastic constants in lysozyme crystals in terms of the sound velocity measurement by pulse echo methods. Tetragonal hen egg-white lysozyme crystals were grown by the concentration gradient method. The crystals were grown in test tubes, with an inner diameter of 8 ㎜ and 80 ㎜ in length, held vertically. The test tubes were kept at 23C for 2 weeks. The maximum size of crystals were 3×3×4 ㎟. The high quality crystals were examined by Laue topography with a water filter using synchrotron radiation. Figure is a X-ray topograph. Several straight screw dislocations were observed. We also determined Burgers vector to be a [110] direction. The measurement of sound velocity was performed by the digital signal processing method. the crystals were placed in stainless steel vessel, which was filled with lysozyme solution used for crystal growth. We observed the longitudinal sound velocity along the [110] direction in the tetragonal is obtained to be 1817 ㎧. Therefore, Young modulus and shear modulus were evaluated to be 2.70 Gpa and 1.02 Gpa, respectively, if we assumed Poisson ratio is 0.33. These results will be discussed at the meeting.

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