• Title/Summary/Keyword: XPS.

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Characteristics of Pd Catalysts for Methane Oxidation (메탄 산화를 위한 Pd 촉매의 특성)

  • Lee, Jin-Man;Yang, O-Bong;Kim, Chun-Yeong;Woo, Seong-Ihl
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.557-562
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    • 1999
  • The reaction properties of Pd. Pd-Ce and Pd-La catalysts supported on ${\gamma}-Al_2O_3$ were investigated in the oxidation reaction of methane($CH_4$) exhausted from the compressed natural gas vehicle in a U-tube flow reactor with gas hourly space velocity of $72,000h^{-1}$. The catalysts were characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), BET surface area and hydrogen chemisorption. Pd catalyst prepared by $Pd(NO_3)_2$ as a palladium precursor and calcined at $600^{\circ}C$ showed the highest activity for a methane oxidation. Catalytic activity of calcined $Pd/{\gamma}-Al_2O_3$ in which most of palladium was converted into palladium oxide species was higher than that of reduced $Pd/{\gamma}-Al_2O_3$ in which most of palladium existed in palladium metal by XRD. As increasing the number of reaction cycles in the wide range of redox, the catalytic activity of $Pd/{\gamma}-Al_2O_3$ was decreased and the highly active window became narrower. Lanthanum oxide promoted Pd catalyst, $Pd/La/{\gamma}-Al_2O_3$ showed enhanced thermal stability compared with $Pd/{\gamma}-Al_2O_3$ even after aging at $1000^{\circ}C$, which was ascribed to the role of La as a promoter to suppress the sintering of palladium metal and ${\gamma}-Al_2O_3$ support. Almost all of methane was removed by the reaction with NO at the redox ratio of 1.2 in case of oxygen excluded steam, but that activity was significantly decreased in the steam containing oxygen.

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Preparation of (n-BuCp)2ZrCl2 Catalyst Supported on SiO2/MgCl2 Binary Support and its Ethylene-1-hexene Copolymerization (SiO2/MgCl2 이원 담체에 담지된 (n-BuCp)2ZrCl2 합성과 에틸렌-1-헥센 공중합)

  • Carino, Ann Charise;Park, Sang Jun;Ko, Young Soo
    • Applied Chemistry for Engineering
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    • v.29 no.4
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    • pp.461-467
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    • 2018
  • In this study, $(n-BuCp)_2ZrCl_2$, was supported on $SiO_2/MgCl_2$ binary support. Before supporting the catalyst, the $SiO_2/MgCl_2$ binary support was surface treated with three different alkyl aluminum compound, namely trimethylaluminum, triethylaluminum, and ethylaluminum sesquichloride. The synthesized surface-treated $SiO_2/MgCl_2$ supported metallocene catalysts were used for the copolymerization of ethylene and 1-hexene. Their catalytic properties and performances were analyzed through BET, XPS analysis, ICP-AES analysis, and FE-SEM. While the resulting copolymers were analyzed through DSC analysis, GPC analysis, 13C-NMR analysis, and FE-SEM. The analysis of synthesized surface-treated $SiO_2/MgCl_2$ supported metallocene catalysts showed that the Zr content of these catalysts is relatively lower compared to that of the catalyst supported on $SiO_2$. This could be attributed to the reduction in the surface area of $SiO_2$ due to the presence of recrystallized $MgCl_2$ and alkyl aluminum. Furthermore, they exhibited a better copolymerization activity compared to that of $SiO_2$ supported catalyst, particularly the EASC-surface treated binary support, which has the highest activity of 1.9 kg PE/($mmol-Zr^*hr$) because EASC acts as a strong Lewis acid. It could also be observed that the larger the ligand of alkyl aluminum used, the rougher the particle surface of the resulting polymer.

Surface characteristics and stability of implants treated with alkali and heat (알칼리와 열처리에 의한 임플란트의 표면 특성 및 골유착 안정성에 관한 연구)

  • Song, Yun-Seok;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.46 no.5
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    • pp.490-499
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    • 2008
  • Statement of problem: Bioactive materials must have the ability to spontaneously form a bone like apatite layer on their surface and induce direct biochemical bonding to bone. A simple chemical treatment via alkali and heat has been revealed to induce bioactivity in titanium. Purpose: The purpose of this study was to evaluate the surface characteristics and stability of alkali and heat treated implants. Material and methods: Specimens were divided into three groups; group 1 was the control group with machined surface implants, groups 2 and 3 were treated with alkali solutions and heat treated in the atmosphere and vacuum conditions respectively. The surface characteristics were observed with FESEM, XPS, TF-XRD and AFM. Stability was evaluated with the resonance frequency analysis, periotest and removal torque values. One-way ANOVA and Duncan test were used for statistical analysis. Results: 1. Groups treated with alkali and heat showed similar characteristics. Groups 2 and 3 showed high compositions of Na ions on the surface with sub-micron sized pores compared to group 1. Group 2 showed mixed compositions of anatase and rutile with superior contents of rutile. 2. Resonance frequency analysis : The ISQ of group 2 showed significantly higher values than that of groups 1 and 3 at 12 weeks. The ISQ of groups 1 and 2 showed significant increase after 4 weeks, and the ISQ of group 3 increased significantly after 2 and 4 weeks respectively (P < .05). 3. Periotest: The PTV of groups 1 and 2 showed significant decrease after 4 weeks, and the PTV of group 3 showed significant decrease after 2 and 4 weeks respectively (P < .05). 4. Removal torque analysis: The removal torque value of group 2 was significantly higher than those of groups 1 and 3 at 2, 4 and 8 weeks. The removal torque values of groups 1 and 3 showed increase at 4 and 12 weeks, but the removal torque value of group 2 showed increase after 4 weeks (P < .05). Conclusion: An oxide layer with appropriate crystal structure and amorphous sodium titanate layer can be obtained on titanium implants through alkali and heat treatment in the atmosphere, and even alkali and heat treatment in vacuum conditions, provided a bioactive surface containing sodium. These surface layers can be considered to be effective for enhancement of osseointegration and reduction of healing period for implant treatment.

Characterization and Conversion Electron Mössbauer Spectroscopy of HoMn1-x-FexO3 Thin Films by Pulsed Laser Deposition (PLD를 이용한 HoMn1-x-FexO3 박막 제조 및 후방 산란형 뫼스바우어 분광 연구)

  • Choi, Dong-Hyeok;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.18-21
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    • 2007
  • The hexagonal $HoMn_{1-x}-Fe_xO_3$(x=0.00, 0.05) thin films were prepared using pulsed laser deposition(PLD) method on $Pt/Ti/SiO_2/Si$ substrate. The microstructure and magnetic properties have been studied by x-ray diffraction(XRD), atomic force microscopy (AFH), scanning electron microscope(SEM:), x-ray photoelectron spectroscopy(XPS), and conversion electron $M\"{o}ssbauer$ spectroscopy(CEMS). From the analysis of the x-ray diffraction patterns, the crystal structure for all films was found to be a hexagonal($P6_3cm$), which was preferentially grown along(110) direction. The lattice constant $c_0$ of the film with x=0.05 was close to that of single crystal, whereas lattice constant $a_0$ with respect to single crystal shows a slight decrease. This difference of lattice parameters between film and single crystal was caused by the lattice mismatch between the film and $Pt/Ti/SiO_2/Si$ substrate. Conversion electron $M\"{o}ssbauer$ spectrum of $HoMn_{0.95}Fe_{0.05}O_3$ thin film shows an asymmetry doublet absorption ratio at room temperature, which is due to the oriented direction of crystallographic domains. This is corresponding with analysis of x-ray diffraction. The quadrupole splitting(${\Delta}E_Q$) at room temperature is found to be $1.62{\pm}0.01mm/s$. This large ${\Delta}E_Q$ was caused by asymmetry environment surrounding Fe ion.

Preparation of Ni-doped Gamma Alumina from Gibbsite and Its Characteristics (깁사이트로부터 니켈피착 감마알루미나의 제조 및 특성)

  • Lee, Hyun;Chung, In-Sung;Park, Hee-Chan
    • Korean Journal of Materials Research
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    • v.8 no.12
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    • pp.1158-1164
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    • 1998
  • Aluminium sulfate solution was prepared by sulfuric acid treatment from gibbsite. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was precipitated from aluminium sulfate solution by adding it into ethylalcohol. From XRD analysis as-prepared $Al_2(SO_4)_3$ · $nH_2O$ was confirmed to have mixed-crystalization water(n=18, 16, 12, 6). The average water of crystalization calculated from thermogravimetry(TG) was 14.7. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was thermally decomposed and converted to $Al_2(SO_4)_3$ at $800^{\circ}C$, $\gamma-Al_2O_3$ at $900-1000^{\circ}C$, and $\alpha-Al_2O_3$ at $1200^{\circ}C$. Ni-doped $\gamma-Al_2O_3$, was synthesized from the slurry of as-prepared $\gamma-Al_2O_3$, with the ratio of [Ni]/[Al]=0.5. The reaction conditions of synthesis were determined as initial pH 9.0 and temperature $80^{\circ}C$ The basicity(pH) of slurry was controlled by using urea and $NH_4OH$ solution. Urea was also used for deposition-precipitation. For determining termination of reaction, the data acquisition was performed by oxidation reduction potential(ORP), conductivity and pH value in the process of reaction. Termination of the reaction was decided by observing the reaction steps and rapid decrease in conductivity. On the other hand, BET(Brunauer, Emmett and Teller) and thermal diffusity of Ni- doped $\gamma-Al_2O_3$, with various content of Ni were measured and compared. Thermal stability of Ni- doped $\gamma-Al_2O_3$ at $1250^{\circ}C$ was confirmed from BET and XRD analysis. The surface state of Ni-doped $\gamma-Al_2O_3$ was investigated by X-ray photoelectron spectroscopy(XPS). The binding energy at $Ni2P_{3/2}$ increased with increasing the formation of $NiAl_2O_4$ phase.

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Effect of SO2 on NOx Removal Performance in Low Temperature Region over V2O5-Sb2O3/TiO2 SCR Catalyst Washcoated on the Metal Foam (저온영역에서 메탈폼에 코팅된 V2O5-Sb2O3/TiO2 SCR 촉매의 NOx 저감성능에 미치는 SO2 영향에 관한 연구)

  • Na, Woo-Jin;Park, Young-Jin;Bang, Hyun-Seok;Bang, Jong-Seong;Park, Hea-Kyung
    • Clean Technology
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    • v.22 no.2
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    • pp.132-138
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    • 2016
  • The emission of SO2 is inevitable in case of combustion of most fossil fuels except LNG in commercial power plant which has a bad effect on the durability of SCR catalyst. To develop a low temperature SCR catalyst which has a high NOx removal performance and excellent durability to SO2, V2O5/TiO2 catalysts were prepared by coating on the metal foam substrate with the impregnation amount of Sb2O3 as promotor. This study has evaluated the NOx removal performance and the durability to SO2 on a laboratory scale atmospheric reactor and analyzed the properties of the prepared catalysts by means of porosimeter, BET, SEM (scanning electron microscope), EDX (energy dispersive x-ray spectrometer), XPS (X-ray photoelectron spectroscopy). It was found that the surface area of catalyst increased with the impregnation amount of Sb2O3 and the NOx removal performance showed the highest value at the 2 wt% impregnation of Sb2O3. This results was considered to be due to the optimum active site on the catalyst surface. And also, Sb2O3 impregnated catalysts presented that NOx removal performance was maintained despite the exposure to SO2 for 5 hours. Therefore it was confirmed that metal foam SCR catalyst for low temperature could be manufactured with the optimum control of Sb2O3 impregnation according to the SO2 presence or not.

Oxidative Desulfurization of Marine Diesel Using Keggin Type Heteropoly Acid Catalysts (Keggin형 헤테로폴리산 촉매를 이용한 선박용 경유의 산화 탈황)

  • Oh, Hyeonwoo;Woo, Hee Chul
    • Clean Technology
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    • v.25 no.1
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    • pp.91-97
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    • 2019
  • Oxidative desulfurization (ODS) has received much attention in recent years because refractory sulfur compounds such as dibenzothiophenes can be oxidized selectively to their corresponding sulfoxides and sulfones, and these products can be removed by extraction and adsorption. In this work, The oxidative desulfurization of marine diesel fuel was performed in a batch reactor with hydrogen peroxide ($H_2O_2$) in the presence of various supported heteropoly acid catalysts. The catalysts were characterized by XRD, XRF, XPS and nitrogen adsorption isotherm techniques. Based on the sulfur removal efficiency of promising silica supported heteropoly acid catalysts, the ranking of catalytic activity was: $30\;H_3PW_{12}/SiO_2$ > $30\;H_3PMo_{12}/SiO_2$ > $30\;H_4SiW_{12}/SiO_2$, which appears to be related with their intrinsic acid strength. The $30\;H_3PW_{12}/SiO_2$ catalyst showed the highest initial sulfur removal efficiency of about 66% under reaction conditions of $30^{\circ}C$, $0.025g\;mL^{-1}$ (cat./oil), 1 h reaction time. However, through the recycle test of the $H_3PW_{12}/SiO_2$ catalyst, significant deactivation was observed, which was attributed to the elution of the active component $H_3PW_{12}$. By introducing cesium cation ($Cs^+$) into the $H_3PW_{12}/SiO_2$ catalyst, the stability of the catalyst was improved with changing the solubility, and the $Cs^+$ ion exchanged catalyst could be recycled for at least five times without severe elution.

Influences of the Composition on Spectroscopic Characteristics of AlxGa1-xN Thin Films (AlxGa1-xN 박막의 조성이 분광학적 특성에 미치는 영향)

  • Kim, Dae Jung;Kim, Bong Jin;Kim, Duk Hyeon;Lee, Jong Won
    • New Physics: Sae Mulli
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    • v.68 no.12
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    • pp.1281-1287
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    • 2018
  • In this study, $Al_xGa_{1-x}N$ films were grown on (0001) sapphire substrates by using metal-organic chemical vapor deposition (MOCVD). The crystallinity of the grown films was examined with X-ray diffraction (XRD) patterns. The surfaces and the chemical properties of the $Al_xGa_{1-x}N$ films were investigated using atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS), respectively. The optical properties of the $Al_xGa_{1-x}N$ film were studied in a wide photon energy range between 2.0 ~ 8.7 eV by using spectroscopic ellipsometry (SE) at room temperature. The data obtained by using SE were analyzed to find the critical points of the pseudodielectric function spectra, $<{\varepsilon}(E)>=<{\varepsilon}_1(E)>+i<{\varepsilon}_2(E)>$. In addition, the second derivative spectra, $d^2<{\varepsilon}(E)>/dE^2$, of the pseudodielectric function for the $Al_xGa_{1-x}N$ films were numerically calculated to determine the critical points (CPs), such as the $E_0$, $E_1$, and $E_2$ structure. For the four samples (x = 0.18, 0.21, 0.25, 0.29) between a composition of x = 0.18 and x = 0.29, changes in the critical points (blue-shifts) with increasing Al composition at 300 K for the $Al_xGa_{1-x}N$ film were observed via ellipsometric measurements for the first time.

Studies on the Varietal Response of Soybeans to Nitrogen Application Level under Different Soil Acidity II. Effect of pH and Nitrogen Application on the Growth and Yield of Soybean Cultivars (대두의 토양산도에 따른 질소반응 연구 II. 토양 및 양액의 산도와 질소시용량에 따른 대두의 생육 및 수량반응)

  • Lee, Hong-Suk;Kwon, Oh-Ha;Ahn, Yong-Tae
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.33 no.2
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    • pp.103-111
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    • 1988
  • This study was carried out with two cultivars under two levels of pH and four levels of nitrogen fertilization in a field and nutri-culture experiments to obtain the information about the effects of pH and nitrogen fertilization on the growth and yield of soybean. Acidic condition suppressed the growth of soybean plants, and thus yield and yield components of soybean decreased under acidic condition. But they increased with increased nitrogen fertilization. Especially, these respones were more remarkable under acidic condition and in the variety Jangbaegkong. Grain yield of soybean were highly correlated with the content of allantoin and total nitrogen of soybean plants in the variety Jangbaegkong, but this was not in the variety Danyeobkong. The content of protein and fat of soybean seeds decreased under acidic condition, and more nitrogen fertilization increased the protein content, but decreased the fat content.

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Deposition of ZnO Thin Films by RF Magnetron Sputtering and Cu-doping Effects (RF 마그네트론 스퍼터링에 의한 ZnO박막의 증착 및 구리 도우핑 효과)

  • Lee, Jin-Bok;Lee, Hye-Jeong;Seo, Su-Hyeong;Park, Jin-Seok
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.49 no.12
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    • pp.654-664
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    • 2000
  • Thin films of ZnO are deposited by using an RF magnetron sputtering with varying the substrate temperature(RT~39$0^{\circ}C$) and RF power(50~250W). Cu-doped ZnO(denoted by ZnO:Cu) films have also been prepared by co-spputtering of a ZnO target on which some Cu-chips are attached. Different substrate materials, such as Si, $SiO_{2}/Si$, sapphire, DLC/Si, and poly-diamond/Si, are employed to compare the c-axial growth features of deposited ZnO films. Texture coefficient(TC) values for the (002)-preferential growth are estimated from the XRD spectra of deposited films. Optimal ranges of RF powers and substrate temperatures for obtaining high TC values are determined. Effects of Cu-doping conditions, such as relative Cu-chip sputtering areas, $O_{2}/(Ar+O_{2})$ mixing ratios, and reactor pressures, on TC values, electrical resistivities, and relative Cu-compositions of deposited ZnO:Cu films have been systematically investigated. XPS study shows that the relative densities of metallic $Cu(Cu^{0})$ atoms and $CuO(Cu^{2+})$-phases within deposited films may play an important role of determining their electrical resistivities. It should be noted from the experimental results that highly resistive(> $10^{10}{\Omega}cm$ ZnO films with high TC values(> 80%) can be achieved by Cu-doping. SAW devices with ZnO(or Zn):Cu)/IDT/$SiO_{2}$/Si configuration are also fabricated to estimate the effective electric-mechanical coupling coefficient($k_{eff}^{2}$) and the insertion loss. It is observed that the devices using the Cu-doped ZnO films have a higher $k_{eff}^{2}$ and a lower insertion loss, compared with those using the undoped films.

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