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

Search Result 2,642, Processing Time 0.031 seconds

Preparation and Gas Permeation Performance of Pd-Ag-Cu Hydrogen Separation Membrane Using α-Al2O3 Support (α-Al2O3 지지체를 이용한 Pd-Ag-Cu 수소 분리막의 제조 및 기체투과 성능)

  • Sung Woo Han;Min Chang Shin;Xuelong Zhuang;Jae Yeon Hwang;Min Young Ko;Si Eun Kim;Chang Hoon Jung;Jung Hoon Park
    • Membrane Journal
    • /
    • v.34 no.1
    • /
    • pp.50-57
    • /
    • 2024
  • In this experiment, Pd-Ag-Cu membrane was manufactured using electroless plating on an α-Al2O3 support. Pd, Ag and Cu were each coated on the surface of the support through electroless plating and heat treatment was performed for 18 h at 500℃ in H2 in the middle of electroless plating to form Pd alloy. The surface of the Pd-Ag-Cu membrane was observed through Scanning Electron Microscopy (SEM), and the thickness of the Pd membrane was measured to be 7.82 ㎛ and the thickness of the Pd-Ag-Cu membrane was measured to be 3.54 ㎛. Energy dispersive X-ray spectroscopy and X-ray diffraction analysis confirmed the formation of a Pd-Ag-Cu alloy with a composition of Pd-78wt%, Ag-8.81wt% and Cu-13.19wt%. The gas permeation experiment was conducted under the conditions of 350~450℃ and 1~4 bar in H2 single gas and H2/N2 mixed gas. The maximum H2 flux of the hydrogen separation membrane measured in H2 single gas is 74.16 ml/cm2·min at 450℃ and 4 bar for the Pd membrane and 113.64 ml/cm2·min at 450℃ and 4 bar for the Pd-Ag-Cu membrane. In the case of the separation factor measured in H2/N2 mixed gas, separation factors of 2437 and 11032 were measured at 450℃ and 4 bar.

Relationship between Physicochemical Properties, Heavy Metal Contents and Magnetic Susceptibility of Soils (토양의 물리화학적 특성, 중금속 함량, 대자율 간의 상호관계 연구)

  • Chon, Chul-Min;Park, Jeong-Sik;Kim, Jae-Gon;Lee, Youn-Soo
    • Journal of the Mineralogical Society of Korea
    • /
    • v.23 no.4
    • /
    • pp.281-295
    • /
    • 2010
  • This paper deals with magnetic susceptibility, mineralogy, soil properties (pH, EC, CEC, loss on ignition), iron and manganese oxides, the content and partitioning of heavy metals (As, Cd, Cr, Cu, Ni, Pb, Zn), and their mutual relationship in the soil samples of an unpolluted, abandoned mine area, and industrial complex area. The various minerals derived from weathered bedrock were identified by X-ray diffraction in the unpolluted soil samples, except for the magnetic minerals. XRD analysis also revealed the existence of hematite and magnetite related to mine tailings and waste rocks in the abandoned mine area samples. The industrial complex area samples had carbonate minerals, such as calcite and dolomite, that might be due to anthropogenic deposition. The sum of the reducible, oxidizable, and residual fractions was over 80% for the abandoned mine area samples and over 50% for the industrial complex area samples using the sequential extraction method. The industrial complex area samples had a relatively high carbonate fraction that was associated with carbonate minerals. The content of aqua regia-extractable Fe, Mn, As, and Zn had a high positive correlation with the content of the dithionite-citrate-bicarbonate (DCB)-extractable method related to Fe/Mn oxide phases. The 54% and 58% of aqua regia-extractable Fe and As content, respectively, acted together with the concentrations of the DCB-extractable phases. Magnetic susceptibility values of total samples ranged from 0.005 to $2.131{\times}10^{-6}m^3kg^{-1}$. The samples including iron oxide minerals, such as hematite and magnetite, had a high magnetic susceptibility. The magnetic susceptibility showed a significant correlation with the heavy metals, Cd (r=0.544, p<0.05), Cr (r=0.714, p<0.01), Ni (r=0.645, p<0.05), Pb (r=0.703, p<0.01), and Zn (r=0.496, p<0.01), as well as Fe (r=0.608, p<0.01) and Mn (r=0.615, p<0.01). The aqua regia-extractable Fe and Mn content had a significant positive correlation with Cd, Cr, Cu, Ni, and Zn. However, the DCB-extractable Fe and Mn content had a significant positive correlation with As and Ni, indicating that the heavy metals were associated with Fe and Mn oxide minerals.

Temperature-Programmed Reduction of Copper Oxide Supported on ${\gamma}-Al_2O_3$ and $SiO_2$ (${\gamma}-Al_2O_3$$SiO_2$에 입혀진 산화 구리의 승온 환원)

  • Hwa-Gyung Lee;Chong-Soo Han;Min-Soo Cho;Kae-Soo Lee;Hakze Chon
    • Journal of the Korean Chemical Society
    • /
    • v.30 no.5
    • /
    • pp.415-422
    • /
    • 1986
  • The metal-support interaction of copper oxide supported on ${\gamma}$-alumina and silica was studied by X-ray diffraction (XRD) and temperature-programmed reduction(TPR). It was found that XRD pattern of CuO can not be observed up to 5.0wt % copper content for CuO/${\gamma}-Al_2O_3$ while CuO/$SiO_2$ sample shows the CuO pattern even at 2.5wt% copper content. $H_2-$TPR of CuO/${\gamma}-Al_2O_3$ system shows four major peaks at 145${\circ}C$, 185${\circ}C$, 210${\circ}C$, and 250${\circ}C$. In the case of CuO/$SiO_2$, a large peak at 250${\circ}C$ was appeared accompanying a small peak at 425${\circ}C$. Comparing the TPR peaks with that of copper aluminate which was prepared from the calcination of CuO/${\gamma}-Al_2O_3$ at 1000${\circ}C$, the peaks at around 145${\circ}C$, 200${\circ}C$ (185${\circ}C$ and 210${\circ}C$), and 250${\circ}C$ were corresponded to $Cu^+$ ion in CuO interacting ${\gamma}-Al_2O_3$, $Cu^+$ ions in defect sites of ${\gamma}-Al_2O_3$ and $Cu^{2+}$ ion in the bulk CuO layer, respectively. From the results, it was concluded that there is considerable metal-support interaction in CuO on ${\gamma}-Al_2O_3$ and the interaction results in a stabilization of $Cu^+$ ion in the system.

  • PDF

Magnetic and Electric Transport Properties of MnTe Thin Film Grown by Molecular Beam Epitaxy (분자선 증착법에 의해 성장한 MnTe 박막의 자기적 및 전기수송 특성)

  • Kim, Woo-Chul;Bae, Sung-Whan;Kim, Sam-Jin;Kim, Chul-Sung;Kim, Kwang-Joo;Yoon, Jung-Bum;Jung, Myung-Hwa
    • Journal of the Korean Magnetics Society
    • /
    • v.17 no.2
    • /
    • pp.81-85
    • /
    • 2007
  • MnTe layers of high crystalline quality were successfully grown on Si(100) : B and Si(111) substrates by molecular beam epitaxy (MBE). Under tellurium-rich condition and the substrate temperature around $400^{\circ}C$, a layer thickness of $700{\AA}$ could be easily obtained with the growth rate of $1.1 {\AA}/s$. We investigated the structural, magnetic and transport properties of MnTe layers by using x-ray diffraction (XRD), superconducting quantum interference device (SQUID) magnetometry, and physical properties measurement system (PPMS). Characterization of MnTe layers on Si(100) : B and Si(111) substrates by XRD revealed a hexagonal structure of polycrystals with lattice parameters, ${\alpha}=4.143{\pm}0.001{\AA}\;and\;c=6.707{\pm}0.001{\AA}$. Investigation of magnetic and transport properties of MnTe films showed anomalies unlike antiferromagnetic powder MnTe. The temperature dependence of the magnetization data taken in zero-field-tooling (ZFC) and field-cooling (FC) conditions indicates three magnetic transitions at around 21, 49, and 210 K as well as the great irreversibility between ZFC and FC magnetization in the films. These anomalies are attributable to a magnetic-elastic coupling in the films. Magnetization measurements indicate ferromagnetic behaviour with hysteresis loops at 5 and 300 K for MnTe polycrystalline film. The coercivity ($H_c$) values at 5 and 300 K are 55 and 44 Oe, respectively. In electro-transport measurements, the temperature dependence of resistivity revealed a noticeable semiconducting behaviours and showed conduction via Mott variable range hopping at low temperatures.

Microbial Leaching of Iron from Magnetite (미생물을 이용한 자철석으로부터 철 침출에 관한 연구)

  • Roh, Yul;Oh, Jong-Min;Seo, Yong-Jae;Jang, Hee-Dong
    • Journal of the Mineralogical Society of Korea
    • /
    • v.19 no.4 s.50
    • /
    • pp.265-275
    • /
    • 2006
  • It is in its infancy to use bacteria as a novel biotechnology for leaching precious and heavy metals from raw materials. The objective of this study was to investigate biogeochemical processes of iron leaching from magnetite reduction by iron-reducing bacteria isolated from intertidal flat sediments, southwestern part of Korea. Microbial leaching experiments were performed using commercial magnetite, Aldrich magnetite, in well-defined mediums with and without bacteria. Water soluble Fe production was determined by ICP analysis of bioleached samples in comparison to uninoculated controls, and the resulting precipitated solids were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The extent of iron leaching from magnetite in the aerobic conditions (Fe = 107 ppm) was higher than that in the anaerobic environments (Fe = 94 ppm). In the anaerobic conditions, Fe(III) in commercial magnetite was also reduced to Fe(II), but no secondary mineral phases were observed. Amorphous iron oxides formed in the medium under aerobic conditions where there was sufficient supply of oxygen from the atmosphere. SEM observation suggests that the reduction process involves dissolution-precipitation mechanisms as opposed to solid state conversion of magnetite to amorphous iron oxides. The ability of bacteria to leach soluble iron and precipitate amorphous iron oxides from crystalline magnetite could have significant implications for biogeochemical processes in sediments where Fe(III) in magnetite plays an important role in the largest pool of electron acceptor as well as the tool as a novel biotechnology for leaching precious and heavy metals from raw materials.

CO2 Sequestration and Utilization of Calcium-extracted Slag Using Air-cooled Blast Furnace Slag and Convert Slag (괴재 및 전로슬래그를 이용한 CO2 저감 및 칼슘 추출 후 슬래그 활용)

  • Yoo, Yeongsuk;Choi, Hongbeom;Bang, Jun-Hwan;Chae, Soochun;Kim, Ji-Whan;Kim, Jin-Man;Lee, Seung-Woo
    • Applied Chemistry for Engineering
    • /
    • v.28 no.1
    • /
    • pp.101-111
    • /
    • 2017
  • Mineral carbonation is a technology in which carbonates are synthesized from minerals including serpentine and olivine, and industrial wastes such as slag and cement, of which all contain calcium or magnesium when reacted with carbon dioxide. This study aims to develop the mineral carbonation technology for commercialization, which can reduce environmental burden and process cost through the reduction of carbon dioxide using steel slag and the slag reuse after calcium extraction. Calcium extraction was conducted using NH4Cl solution for air-cooled slag and convert slag, and ${\geq}98%$ purity calcium carbonate was synthesized by reaction with calcium-extracted solution and carbon dioxide. And we conducted experimentally to minimize the quantity of by-product, the slag residue after calcium extraction, which has occupied large amount of weight ratio (about 80-90%) at the point of mineral carbonation process using slag. The slag residue was used to replace silica sand in the manufacture of cement panel, and physical properties including compressive strength and flexible strength of panel using the slag residue and normal cement panel, respectively, were analyzed. The calcium concentration in extraction solution was analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES). Field-emission scanning electron microscope (FE-SEM) was also used to identify the surface morphology of calcium carbonate, and XRD was used to analyze the crystallinity and the quantitative analysis of calcium carbonate. In addition, the cement panel evaluation was carried out according to KS L ISO 679, and the compressive strength and flexural strength of the panels were measured.

Pressure-load Calibration of Multi-anvil Press and the Thermal Gradient within the Sample Chamber (멀티 앤빌 프레스의 압력-부하 보정 작업과 시료 내의 온도구배 연구)

  • Kim, Eun Jeong;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
    • /
    • v.31 no.3
    • /
    • pp.161-172
    • /
    • 2018
  • Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.

Glycerol Steam Reforming for Hydrogen Production on Metal-ceramic Core-shell CoAl2O4@Al Composite Structures (금속-세라믹 Core-Shell CoAl2O4@Al 구조체를 적용한 불균일계 촉매의 글리세롤 수소전환 반응특성)

  • Kim, Jieun;Lee, Doohwan
    • Clean Technology
    • /
    • v.21 no.1
    • /
    • pp.68-75
    • /
    • 2015
  • In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl2O4@Al micro-composite for heterogeneous catalysts support. The CoAl2O4@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl2O4 shell. For comparison, CoAl2O4 was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl2O4@Al and CoAl2O4 were prepared by incipient wetness impregnation and characterized by N2 adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl2O4@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl2O4 due to facilitated heat transport through the core-shell structure. The CoAl2O4@Al and CoAl2O4 also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl2O4@Al core-shell than CoAl2O4. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.

Ti-Getter Effects on Magnetic Properties of Ti0.96Co0.02Fe0.02O2 (Ti-Getter가 Ti0.96Co0.02Fe0.02O2의 자기적 특성에 미치는 영향)

  • Nam, H.D.;Kim, S.J.;Baek, J.K.;Lee, S.R.;Park, Cheol-Su;Kim, E.C.
    • Journal of the Korean Magnetics Society
    • /
    • v.18 no.3
    • /
    • pp.109-114
    • /
    • 2008
  • The samples were synthesized by using a solid state reaction. The X-ray diffraction pattern for $Ti_{0.96}Co_{0.02}Fe_{0.02}O_2$ showed a pure rutile phase with tetragonal structure, Mixtures of the proper proportions of the elements sealed in evacuated quartz ampoule were heated at $870{\sim}930^{\circ}C$ for one day and then slowly cooled down to room temperature at a rate of $10^{\circ}C$/h. In order to obtain single phase material, it was necessary to grind the sample after the first firing and to press the powders into pellets before annealing them for a second time in evacuated and sealed quartz ampoule. Magnetic properties have been investigated using the vibrating sample magnetometer (VSM). Room temperature magnetic hysteresis (M-H) curve showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $1.5\;{\mu}_B$/CoFe. But the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $0.02\;{\mu}_B$/CoFe without Ti-getter. Size of particles is about $1\;{\mu}m$ using the transmission electron microscope (TEM). The ingredients of sample are distributed irregular in particles. Only Fe get shown on the surface of particles.

The Development of an Electroconductive SiC-ZrB2 Composite through Spark Plasma Sintering under Argon Atmosphere

  • Lee, Jung-Hoon;Ju, Jin-Young;Kim, Cheol-Ho;Park, Jin-Hyoung;Lee, Hee-Seung;Shin, Yong-Deok
    • Journal of Electrical Engineering and Technology
    • /
    • v.5 no.2
    • /
    • pp.342-351
    • /
    • 2010
  • The SiC-$ZrB_2$ composites were fabricated by combining 30, 35, 40, 45 and 50 vol. % of zirconium diboride ($ZrB_2$) powders with silicon carbide (SiC) matrix. The SiC-$ZrB_2$ composites and the sintered compacts were produced through spark plasma sintering (SPS) under argon atmosphere, and its physical, electrical, and mechanical properties were examined. Also, the thermal image analysis of the SiC-$ZrB_2$ composites was examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed via x-ray diffraction (XRD) analysis. The apparent porosity of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$, SiC+45vol.%$ZrB_2$ and SiC+50vol.%$ZrB_2$ composites were 7.2546, 0.8920, 0.6038, 1.0981, and 10.0108%, respectively. The XRD phase analysis of the sintered compacts demonstrated a high phase of SiC and $ZrB_2$. Among the $SiC+ZrB_2$ composites, the SiC+50vol.%$ZrB_2$ composite had the lowest flexural strength, 290.54MPa, the other composites had more than 980MPa flexural strength except the SiC+30vol.%$ZrB_2$ composite; the SiC+40vol.%$ZrB_2$ composite had the highest flexural strength, 1011.34MPa, at room temperature. The electrical properties of the SiC-$ZrB_2$ composites had positive temperature coefficient resistance (PTCR). The V-I characteristics of the SiC-$ZrB_2$ composites had a linear shape in the temperature range from room to $500^{\circ}C$. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ SiC+45vol.%$ZrB_2$ and SiC+50vol.%$ZrB_2$ composites were $4.573\times10^{-3}$, $1.554\times10^{-3}$, $9.365\times10^{-4}$, $6.999\times10^{-4}$, and $6.069\times10^{-4}\Omega{\cdot}cm$, respectively, at room temperature, and their resistance temperature coefficients were $1.896\times10^{-3}$, $3.064\times10^{-3}$, $3.169\times10^{-3}$, $3.097\times10^{-3}$, and $3.418\times10^{-3}/^{\circ}C$ in the temperature range from room to $500^{\circ}C$, respectively. Therefore, it is considered that among the sintered compacts the SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ and SiC+45vol.%$ZrB_2$ composites containing the most outstanding mechanical properties as well as PTCR and V-I characteristics can be used as an energy friendly ceramic heater or ohmic-contact electrode material through SPS.