• Title/Summary/Keyword: high temperature X-ray diffraction

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Pt Coating on Flame-Generated Carbon Particles (화염법을 이용한 Pt/C 촉매 제조)

  • Choi, In-Dae;Lee, Dong-Geun
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.33 no.2
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    • pp.116-123
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    • 2009
  • Carbon black, activated carbon and carbon nanotube have been used as supporting materials for precious metal catalysts used in fuel cell electrodes. One-step flame synthesis method is used to coat 2-5nm Pt dots on flame-generated carbon particles. By adjusting flame temperature, gas flow rates and resident time of particles in flame, we can obtain Pt/C nano catalyst-support composite particles. Additional injection of hydrogen gas facilitates pyrolysis of Pt precursor in flame. The size of as-incepted Pt dots increases along the flame due to longer resident time and sintering in high temperature flame. Surface coverage and dispersion of the Pt dots is varied at different sampling heights and confirmed by Transmission electron microscopy (TEM), Energy-dispersive spectra (EDS) and X-ray diffraction (XRD). Crystalinity and surface bonding groups of carbon are investigated through X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy.

Phase Transition of Zeolite X under High Pressure and Temperature (고온 고압 환경에서 합성 제올라이트 X의 상전이 비교연구)

  • Hyunseung Lee;Soojin Lee;Yongmoon Lee
    • Economic and Environmental Geology
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    • v.56 no.1
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    • pp.13-21
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    • 2023
  • X-ray powder diffraction study was conducted on the bulk modulus and phase transition behavior of synthetic zeolite X under high temperature and high pressure. Water and HCO3- solution were used as a PTM. Sample was heated and pressurized up to 250 ℃ and 5.18 GPa. The change of unit cell volume and phase transition were observed by X-ray diffraction. The lattice constants and unit cell volume of zeolite X, gmelinite, natrolite, and smectite were calculated using the GSAS2 program to which Le Bail's whole powder pattern decomposition (WPPD) method was applied. The bulk modulus of each zeolite X and smectite were calculated using the EosFit program to which the Birch-Murnaghan equation was applied. The bulk modulus of zeolite X is 89(3) GPa in water run, and zeolite X is 92(3) GPa in HCO3- solution run. In both run, pressure induced hydration (PIH) occurred due to the inflow of PTM into the zeolite X framework at initial pressure. Zeolite X transited to gmelinite, natrolite, and smectite in water run. Zeolite X, however, transited to smectite in HCO3- solution run. Interzeolite transformation occurred in water run, and did not occur in HCO3- solution run, which is assumed that conflict between the environment to form zeolite and the pH of the HCO3- solution.

Estimation Study of Firing Temperature for Fired Clay Brick Relics Excavated from Buddhist Temple in Karatepa Using Analytical Method of High Temperature X-ray Diffraction (고온 XRD 분석법을 이용한 카라테파 불교사원 출토 점토벽돌의 소성온도 추정연구)

  • Han, Min Su;Lee, Jang Jon;Kim, Jae Hwan
    • Journal of Conservation Science
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    • v.32 no.4
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    • pp.511-520
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    • 2016
  • The purpose of this study was to estimate the firing temperature of fired clay brick by applying high temperature X-ray diffraction(XRD) analysis. The clay bricks, which were excavated from a Buddhist temple in Karatepa, Uzbekistan were composed of quartz, plagioclase, alkali feldspar, mica, chlorite, limestone, hornblende, etc. Some clay bricks contained gypsum, which was presumed to have been used to improve the adhesive strength of the brick. Estimating the firing temperature using a geologic thermometer, the UZ-1 sample was identified as being in the quartz, plagioclase, pyroxene series, and the firing temperature was estimated to be $900-1200^{\circ}C$. On the other hand, applying the high temperature XRD method to the UZ-5 sample, it was found that the limestone was destroyed at $1000^{\circ}C$ and the diffraction peak of chlorite was weakened at $1050^{\circ}C$. Moreover, pyroxene series minerals developed at $1050^{\circ}C$ in the reproduction experiment. These results indicate that the clay bricks used in the temple were produced in a kiln that reached a temperature of more than $1000^{\circ}C$. Thus, high temperature XRD analysis can more accurately estimate firing temperatures as compared to the firing temperature mineral identification method and it can be used to determine the creation and extinction temperature range of minerals.

CuPt-type ordering in Zn-rich $Cd_xZn_{1-x}$Te epilayers grown on GaAs and ZnTe/GaAs (GaAs, ZnTe/GaAs 기판위 성장된 고농도 Zn 조성의 $Cd_xZn_{1-x}$Te 에피층에서의 CuPt형 나노 규칙상 형성)

  • 권명석
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.5
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    • pp.230-234
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    • 2003
  • CuPt-type ordering has been observed in Zn-rich $Cd_xZn_{1-x}$Te epilayers grown on (001)GaAs and ZnTe/GaAs(001) substrates. X-ray diffraction, electron beam diffraction, high-resolution transmission electron microscopy and low-temperature photoluminescence have been used to characterize the CuPt-type ordering in Zn-rich $Cd_xZn_{1-x}$Te epilayers.

Effect of DyFeO3 Addition on Crystal Structure and Ferrcelectricity of the BiFeO3-PbTiO3 System

  • Kim, Seong-Seog;Kwon, Jong-Uk;Cheon, Chae Il
    • Journal of the Korean Ceramic Society
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    • v.42 no.5 s.276
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    • pp.299-303
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    • 2005
  • The crystal structure and ferroelectricity of the $(1-x)BiFeO_3\;(BF)-xPbTiO_3$ (PT) ceramic system with the addition of $DyFeO_3$ (DF) have been investigated for attaining a high temperature piezoelectric material. This study is focused on the relation between crystal structure and ferroelectric property with the addition of DF over the phase boundary in the (1-x)BF-xPT system. Hysteresis curves of polarization-electric field at room temperature have been measured. The X-ray and neutron diffraction data were analyzed by the rietveld refinement method. The addition of 0.1 mole DF into BF-PT system greatly increases the ferroelectric remanant polarization Pr values, e.g. 17 ${\mu}C/cm^2$ in 0.6BF-yDF-(0.4-y)PT and 31${\mu}C/cm^2$ in 0.5BF-yDF-(0.5.y)PT, respectively. The improved Pr value has been discussed in relation with crystal structure and electrical property.

Analysis of the Change in Microstructures of Nano Copper Powders During the Hydrogen Reduction using X-ray Diffraction Patterns and Transmission Electron Microscope, and the Mechanical Property of Compacted Powders (X-선 회절 패턴 측정과 투과 전자 현미경을 이용한 구리 나노분말의 수소 환원 처리 시 발생하는 미세조직 변화 및 치밀화 시편의 물성 분석)

  • Ahn, Dong-Hyun;Lee, Dong Jun;Kim, Wooyeol;Park, Lee Ju;Kim, Hyoung Seop
    • Journal of Powder Materials
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    • v.21 no.3
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    • pp.207-214
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    • 2014
  • In this study, nano-scale copper powders were reduction treated in a hydrogen atmosphere at the relatively high temperature of $350^{\circ}C$ in order to eliminate surface oxide layers, which are the main obstacles for fabricating a nano/ultrafine grained bulk parts from the nano-scale powders. The changes in composition and microstructure before and after the hydrogen reduction treatment were evaluated by analyzing X-ray diffraction (XRD) line profile patterns using the convolutional multiple whole profile (CMWP) procedure. In order to confirm the result from the XRD line profile analysis, transmitted electron microscope observations were performed on the specimen of the hydrogen reduction treated powders fabricated using a focused ion beam process. A quasi-statically compacted specimen from the nano-scale powders was produced and Vickers micro-hardness was measured to verify the potential of the powders as the basis for a bulk nano/ultrafine grained material. Although the bonding between particles and the growth in size of the particles occurred, crystallites retained their nano-scale size evaluated using the XRD results. The hardness results demonstrate the usefulness of the powders for a nano/ultrafine grained material, once a good consolidation of powders is achieved.

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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Effects of Ni Addition on the Microstructures and Magnetic Properties of Fe70-xPd30Nix High-Temperature Ferromagnetic Shape Memory Alloys

  • Lin, Chien-Feng;Yang, Jin-Bin
    • Journal of Magnetics
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    • v.17 no.2
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    • pp.86-95
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    • 2012
  • This study investigated the effects of adding a third alloying element, Ni, to create $Fe_{70-x}Pd_{30}Ni_x$ (x = 2, 4, 6, 8 at.% Ni) ferromagnetic shape memory alloys (FSMAs). The Ni replaced a portion of the Fe. The $Fe_{70-x}Pd_{30}Ni_x$ alloys were homogenized through hot and cold forging to gain a ~38% reduction in thickness, next they were solution-treated (ST) with annealing recrystallization at $1100^{\circ}C$ for 8 h and quenched in ice brine, and then aged at $500^{\circ}C$ for 100 h. Investigation of the microstructures and magnetostriction indicated that the greater Ni amount in the $Fe_{70-x}Pd_{30}Ni_x$ alloys reduced saturation magnetostriction at room temperature (RT). It was also observed that it was more difficult to generate annealed recrystallization. However, with greater Ni addition into the $Fe_{70-x}Pd_{30}Ni_x$ (x = 6, 8 at.% Ni) alloys, the $L1_0+L1_m$ twin phase decomposition into stoichiometric $L1_0+L1_m+{\alpha}_{bct}$ structures was suppressed after the $500^{\circ}C$/100 h aging treatment. The result was that the $Fe_{70-x}Pd_{30}Ni_x$ (x = 6, 8 at.% Ni) alloys maintained a high magnetostriction and magnetostrictive susceptibility (${\Delta}{\lambda}{_\parallel}{^s}/{\Delta}H$) after the alloys were aged at $500^{\circ}C$ for 100 h. This magnetic property of the $Fe_{70-x}Pd_{30}Ni_x$ (x = 6, 8 at.% Ni) alloys make it suitable for application in a high temperature (T > $500^{\circ}C$) and high frequency environments.

Microwave Dielectric Properties of the (l-x)$TiTe_3O_{8}$-x$MgTiO_3$ Ceramics with Sintering Temperature (소결온도에 따른 (l-x)$TiTe_3O_{8}$-x$MgTiO_3$ 세라믹스의 마이크로파 유전 특성)

  • 최의선;김재식;이문기;류기원;이영희
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.53 no.9
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    • pp.459-463
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    • 2004
  • In this study, the (l-x)$TiTe_3O_{8}$-x$MgTiO_3$ ceramics were investigated to obtain the improved dielectric properties of a high temperature stability and a sintering temperature of less than $900^{\circ}C$ which was necessary for the LTCC. According to the X-ray diffraction patterns of the (l-x)$TiTe_3O_{8}$-x$MgTiO_3$(x=0∼1) ceramics, the columbite structure of $TiTe_3O_{8}$ and ilmenite structure of $MgTiO_3$ were coexisted. Increasing the $MgTiO_3$ mole ratio(x), the density and dielectric constant were decreased and temperature coefficient of resonant frequency was moved to the negative direction and the quality factor was increased. In the case of the 0.6$TiTe_3O_{8}$-0.4$MgTiO_3$ ceramics sintered at $830^{\circ}C$ for 3hr., the microwave dielectric properties were $\varepsilon_{\gamma}$=29.3, Q${\times}$$f_{\gamma}$=39.600GHz and $\tau$$_{f}$=+9.3ppm/$^{\circ}C$.

The synthesis of Highly Crystalline and monodisperse maghemite and zirconia Nanocrystallites without size-selection process

  • Park, Jong-Nam;Joo, Jin;Yoo, Tae-kyung;Na, Hyun-Bin;Lee, Soo-Sung;Park, Hyun-Min;Kim, Young-Woon;Hyun, Taek-Hwan
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2003.05a
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    • pp.20-20
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    • 2003
  • A new and simple method has been developed to synthesize highly crystalline and monodisperse maghemite (γ-Fe₂O₃) and zirconia (ZrO₂) nanocristallites. High temperature aging of metal-surfactant complex was founded to generate monodisperse nanoparticles, wherein the nuclei were prepared by the thermal decomposition of iron-oleate complex in case of iron oxide and nonhydrolytic sol-gel reaction in case of zirconia respectively. By varying the experimental conditions, in other words concentration of surfactants, kind of metal precursor, reaction temperature and so on, the diameter of spherical nanoparticles could be controlled at various size. The synthesized nanoparticles were characterized by electron diffraction, X-ray diffraction, and low- and high-resolution transmission electron microscope.

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