• Title/Summary/Keyword: Photoelectron spectroscopy

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Photodecomposition of Concentrated Ammonia over Nanometer-sized TiO2, V-TiO2, and Pt/V-TiO2 Photocatalysts

  • Choi, Hyung-Joo;Kim, Jun-Sik;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.581-588
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    • 2007
  • To enhance the photodecomposition of concentrated ammonia into N2, Pt/V-TiO2 photocatalysts were prepared using solvothermal and impregnation methods. Nanometer-sized particles of 0.1, 0.5 and 1.0 mol% V-TiO2 were prepared solvothermally, and then impregnated with 1.0 wt% Pt. The X-ray diffraction (XRD) peaks assigned to V2O5 at 30.20 (010) and Pt metal at 39.80 (111) and 46.20 (200) were seen in the 1.0 wt% Pt/ 10.0 mol% V-TiO2. The particle size increased in the order: pure TiO2, V-TiO2 and Pt/V-TiO2 after thermal treatment at 500 °C, while their surface areas were in the reverse order. On X-ray photoelectron spectroscopy (XPS), the bands assigned to the Ti2p3/2 and Ti2p1/2 of Ti4+-O were seen in all the photocatalysts, and the binding energies increased in the order: TiO2 < Pt/V-TiO2 < V-TiO2. The XPS bands assigned to the V2p3/2 (517.85, 519.35, and 520.55 eV) and V2p1/2 (524.90 eV) in the V3+, V4+ and V5+ oxides appeared over V-TiO2, respectively, while the band shifted to a lower binding energy with Pt impregnation. The Pt components of Pt/ V-TiO2 were identified at 71.60, 73.80, 75.00 and 76.90 eV, which were assigned to metallic Pt 4f7/2, PtO 4f7/2, PtO2 4f7/2, and PtO 4f5/2, respectively. The UV-visible absorption band shifted closer towards the visible region of the spectrum in V-TiO2 than in pure TiO2 and; surprisingly, the Pt/V-TiO2 absorbed at all wavelengths from 200 to 800 nm. The addition of vanadium generated a new acid site in the framework of TiO2, and the medium acidic site increased with Pt impregnation. The NH3 decomposition increased with the amount of vanadium compared to pure TiO2, and was enhanced with Pt impregnation. NH3 decomposition of 100% was attained over 1.0 wt% Pt/1.0 mol% V-TiO2 after 80 min under illumination with 365 nm light, although about 10% of the ammonia was converted into undesirable NO2 and NO. Various intermediates, such as NO2, -NH2, -NH and NO, were also identified in the Fourier transform infrared (FT-IR) spectra. From the gas chromatography (GC), FT-IR and GC/mass spectroscopy (GC/MS) analyses, partially oxidized NO and NO2 were found to predominate over V-TiO2 and pure TiO2, respectively, while both molecules were reduced over Pt/V-TiO2.

Annealing Effect on Magneto-transport Properties of Amorphous Ge1-xMnx Semiconductor Thin Films (비정질 Ge1-xMnx 박막의 자기수송특성에 미치는 열처리 효과)

  • Kim, Dong-Hwi;Lee, Byeong-Cheol;Lan Anh, Tran Thi;Ihm, Young-Eon;Kim, Do-Jin;Kim, Hyo-Jin;Yu, Sang-Soo;Baek, Kui-Jong;Kim, Chang-Soo
    • Journal of the Korean Magnetics Society
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    • v.19 no.4
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    • pp.121-125
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    • 2009
  • Amorphous $Ge_1$_$_xMn_x$ semiconductor thin films grown by low temperature vapor deposition were annealed at various temperatures from 400 to $700^{\circ}C$ for 3 minutes in high vaccum chamber. The electrical and magnetotransport properties of as-grown and annealed samples have been studied. X-ray diffraction patterns analysis revealed that the samples still maintain amorphous state after annealling at $500^{\circ}C$ for 3 minutes and they were crystallized when annealing temperature increase to $600^{\circ}C$. Temperature dependence of resistivity measurement implied that as-grown and annealed $Ge_1$_$_xMn_x$ films have semiconductor characteristics, the increase of resistivity with annealling temperature was obseved. The $700^{\circ}C$-annealed sample exhibited negative magnetoresistance (MR) at low temperatures and the MR ratio was ${\sim}$8.5% at 10 K. The asymmetry was present in all MR curves. The anomalous Hall Effect was also observed at 250 K.

The surface kinetic properties between $BCl_3/Cl_2$/Ar plasma and $Al_2O_3$ thin film

  • Yang, Xue;Kim, Dong-Pyo;Um, Doo-Seung;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.169-169
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    • 2008
  • To keep pace with scaling trends of CMOS technologies, high-k metal oxides are to be introduced. Due to their high permittivity, high-k materials can achieve the required capacitance with stacks of higher physical thickness to reduce the leakage current through the scaled gate oxide, which make it become much more promising materials to instead of $SiO_2$. As further studying on high-k, an understanding of the relation between the etch characteristics of high-k dielectric materials and plasma properties is required for the low damaged removal process to match standard processing procedure. There are some reports on the dry etching of different high-k materials in ICP and ECR plasma with various plasma parameters, such as different gas combinations ($Cl_2$, $Cl_2/BCl_3$, $Cl_2$/Ar, $SF_6$/Ar, and $CH_4/H_2$/Ar etc). Understanding of the complex behavior of particles at surfaces requires detailed knowledge of both macroscopic and microscopic processes that take place; also certain processes depend critically on temperature and gas pressure. The choice of $BCl_3$ as the chemically active gas results from the fact that it is widely used for the etching o the materials covered by the native oxides due to the effective extraction of oxygen in the form of $BCl_xO_y$ compounds. In this study, the surface reactions and the etch rate of $Al_2O_3$ films in $BCl_3/Cl_2$/Ar plasma were investigated in an inductively coupled plasma(ICP) reactor in terms of the gas mixing ratio, RF power, DC bias and chamber pressure. The variations of relative volume densities for the particles were measured with optical emission spectroscopy (OES). The surface imagination was measured by AFM and SEM. The chemical states of film was investigated using X-ray photoelectron spectroscopy (XPS), which confirmed the existence of nonvolatile etch byproducts.

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Preparation and characterization of Ga-doped TiO2 nanofibers by electrospinning (전기방사를 이용한 Ga이 첨가된 나노섬유의 제작 및 특성평가)

  • Song, Chan-Geun;Kang, Won Ho;Yoon, Jong-Won
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.6
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    • pp.274-278
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    • 2012
  • $TiO_2$ can be used optically and is applied on many areas such as gas sensor, solar cell and photocatalysis. Electrospun nanofibers have received great interest for development and utilization in some novel applications, such as chemical sensors, dye-sensitized solar cell and photo catalysis. In this study, pure $TiO_2$ and Ga-doped $TiO_2$ nanofibers synthesized by a modified electrospinning method. The Ga doped $TiO_2$ solution is prepared by mixing poly vinyl pyrrolidone, ethyl alcohol, and titanium (IV) isopropoxide. By electrospinning these sols, nanofibers were fabricated. These fibers are heat-treated at $800^{\circ}C$ in air. The prepared pure $TiO_2$ and Ga-doped $TiO_2$ nanofibers samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy.

Preparation of Al2O3 Thin Films by Atomic Layer Deposition Using Dimethylaluminum Isopropoxide and Water and Their Reaction Mechanisms

  • An, Ki-Seok;Cho, Won-Tae;Sung, Ki-Whan;Lee, Sun-Sook;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1659-1663
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    • 2003
  • $Al_2O_3$ thin films were grown on H-terminated Si(001) substrates using dimethylaluminum isopropoxide [DMAl: $(CH_3)_2AlOCH(CH_3)_2$], as a new Al precursor, and water by atomic layer deposition (ALD). The selflimiting ALD process by alternate surface reactions of DMAI and $H_2O$ was confirmed from measured thicknesses of the aluminum oxide films as functions of the DMAI pulse time and the number of DMAI-$H_2O$ cycles. Under optimal reaction conditions, a growth rate of ~1.06 ${\AA}$ per ALD cycle was achieved at the substrate temperature of $150\;^{\circ}C$. From a mass spectrometric study of the DMAI-$D_2O$ ALD process, it was determined that the overall binary reaction for the deposition of $Al_2O_3\;[2\;(CH_3)_2AlOCH(CH_3)_2\;+\;3\;H_2O\;{\rightarrow}\;Al_2O_3\;+\;4\;CH_4\;+\;2\;HOCH(CH_3)_2]$can be separated into the following two half-reactions: where the asterisks designate the surface species. Growth of stoichiometric $Al_2O_3$ thin films with carbon incorporation less than 1.5 atomic % was confirmed by depth profiling Auger electron spectroscopy. Atomic force microscopy images show atomically flat and uniform surfaces. X-ray photoelectron spectroscopy and cross-sectional high resolution transmission electron microscopy of an $Al_2O_3$ film indicate that there is no distinguishable interfacial Si oxide layer except that a very thin layer of aluminum silicate may have been formed between the $Al_2O_3$ film and the Si substrate. C-V measurements of an $Al_2O_3$ film showed capacitance values comparable to previously reported values.

Effect of Al2O3 Inter-Layer Grown on FeCrAl Alloy Foam to Improve the Dispersion and Stability of NiO Catalysts (NiO 촉매의 분산성 및 안정성 향상을 위하여 FeCrAl 합금 폼 위에 성장된 Al2O3 Inter-Layer 효과)

  • Lee, Yu-Jin;Koo, Bon-Ryul;Baek, Seong-Ho;Park, Man-Ho;Ahn, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.25 no.8
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    • pp.391-397
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    • 2015
  • NiO catalysts/$Al_2O_3$/FeCrAl alloy foam for hydrogen production was prepared using atomic layer deposition (ALD) and subsequent dip-coating methods. FeCrAl alloy foam and $Al_2O_3$ inter-layer were used as catalyst supports. To improve the dispersion and stability of NiO catalysts, an $Al_2O_3$ inter-layer was introduced and their thickness was systematically controlled to 0, 20, 50 and 80 nm using an ALD technique. The structural, chemical bonding and morphological properties (including dispersion) of the NiO catalysts/$Al_2O_3$/FeCrAl alloy foam were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy and scanning electron microscopy-energy dispersive spectroscopy. In particular, to evaluate the stability of the NiO catalysts grown on $Al_2O_3$/FeCrAl alloy foam, chronoamperometry tests were performed and then the ingredient amounts of electrolytes were analyzed via inductively coupled plasma spectrometer. We found that the introduction of $Al_2O_3$ inter-layer improved the dispersion and stability of the NiO catalysts on the supports. Thus, when an $Al_2O_3$ inter-layer with a 80 nm thickness was grown between the FeCrAl alloy foam and the NiO catalysts, it indicated improved dispersion and stability of the NiO catalysts compared to the other samples. The performance improvement can be explained by optimum thickness of $Al_2O_3$ inter-layer resulting from the role of a passivation layer.

Studies on Thermal and Dynamic Viscoelastic Behaviors of Multiwalled Carbon Nanotubes-reinforced Epoxy Matrix Composites (다중벽 탄소나노튜브강화 에폭시 매트릭스 복합재료의 열적 및 동적 점탄성 거동 연구)

  • Seo, Min-Kang;Park, Soo-Jin
    • Korean Chemical Engineering Research
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    • v.43 no.3
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    • pp.401-406
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    • 2005
  • In this work, the effect of chemical treatment of multiwalled carbon nanotubes (MWNTs) on glass transition temperature (Tg), thermal stability, and dynamic viscoelastic behaviors of MWNTs-reinforced epoxy matrix composites has been studied by differencial scanning calorimeter (DSC), thermogravimetric analysis (TGA), and dynamic mechanical analysis (DMA) measurements. The MWNTs were chemically treated with 35 wt% $H_3PO_4$ (A-MWNTs) or 35 wt% KOH (B-MWNTs) solutions and the changes of surface properties of chemically treated MWNTs were examined by pH, acid and base values, Fourier transfer-infrared spectroscopy (FT-IR), and x-ray photoelectron spectroscopy (XPS) analyses. The chemical treatments based on acid and base reactions led to a significant change of surface characteristics and chemical compositions of the MWNTs, especially A-MWNTs/epoxy composites had higher thermal stability and dynamic viscoelastic properties than those of B-MWNTs and non-treated MWNTs/epoxy composites. These results were probably due to the improvement of interfacial bonding strength, resulting from the acid-base interaction and hydrogen bonding between the epoxy resins and the MWNT fillers.

Selective Oxidation of Single Crystalline AlAs layer on GaAs substrate and XPS(X-ray photoelectron spectroscopy) Analysis (GaAs 기판위에 성장된 단결정 AlAs층의 선택적 산화 및 XPS (X-ray photonelectron spectroscopy) 분석)

  • Lee, Suk-Hun;Lee, Young-Soo;Tae, Heung-Sik;Lee, Young-Hyun;Lee, Jung-Hee
    • Journal of Sensor Science and Technology
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    • v.5 no.5
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    • pp.79-84
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    • 1996
  • A $1\;{\mu}m$ thick n-type GaAs layer with Si doping density of $1{\times}10^{17}/cm^{3}$ and a $500{\AA}$ thick undoped single crystalline AlAs layer were subsequently grown by molecular beam epitaxy on the $n^{+}$ GaAs substrate. The AlAs/GaAs layer was oxidized in $N_{2}$ bubbled $H_{2}O$ vapor($95^{\circ}C$) ambient at $400^{\circ}C$ for 2 and 3 hours. From the result of XPS analysis, small amounts of $As_{2}O_{3}$, AlAs, and elemental As were found in the samples oxidized up to 2 hours. After 3 hours oxidation, however, various oxides related to As were dissolved and As atoms were diffused out toward the oxide surface. The as-grown AlAs/GaAs layer was selectively converted to $Al_{2}O_{3}/GaAs$ at the oxidation temperature $400^{\circ}C$ for 3 hours. The oxidation temperature and time is very critical to stop the oxidation at the AlAs/GaAs interface and to form a defect-free surface layer.

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Effect of Deposition Temperature on the Characteristics of Low Dielectric Fluorinated Amorphous Carbon Thin Films (증착온도가 저유전 a-C:F 박막의 특성에 미치는 영향)

  • Park, Jeong-Won;Yang, Sung-Hoon;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.9 no.12
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    • pp.1211-1215
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    • 1999
  • Fluorinated amorphous carbon (a-C:F) films were prepared by an electron cyclotron resonance chemical vapor deposition (ECRCVD) system using a gas mixture of $C_2F_6$ and $CH_4$ over a range of deposition temperature (room temperature ~ 300$^{\circ}C$). 500$^{\AA}C$ thick DLC films were pre-deposited on Si substrate to improve the strength between substrate and a-C:F film. The chemical bonding structure, chemical composition, surface roughness and dielectric constant of a-C:F films deposited by varying the deposition temperature were studied with a variety of techniques, such as Fourier transform infrared spectroscopy(FTIR), X-ray photoelectron spectroscopy(XPS), atomic force microscopy (AFM) and capacitance-voltage(C-V) measurement. Both deposition rate and fluorine content decreased linearly with increasing deposition temperature. As the deposition temperature increased from room temperature to 300$^{\circ}C$, the fluorine concentration decreased from 53.9at.% down to 41.0at.%. The dielectric constant increased from 2.45 to 2.71 with increasing the deposition temperature from room temperature to 300$^{\circ}C$. The film shrinkage was reduced with increasing deposition temperature. This results ascribed by the increased crosslinking in the films at the higher deposition temperature.

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Adsorption Characteristics of Carbon Dioxide on Chitosan/Zeolite Composites (키토산/제올라이트 복합체의 이산화탄소 흡착 특성)

  • Hong, Woong-Gil;Hwang, Kyung-Jun;Jeong, Gyeong-Won;Yoon, Soon-Do;Shim, Wang Geun
    • Applied Chemistry for Engineering
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    • v.31 no.2
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    • pp.179-186
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    • 2020
  • In this study, chitosan/zeolite composites were prepared by using basalt-based zeolite impregnated with aqueous chitosan solution for the adsorptive separation of CO2. The prepared composites were characterized by scanning electron microscopy (SEM), Fourier-transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), and nitrogen adsorption analysis. In addition, the adsorption equilibrium isotherms for CO2 and N2 were measured at 298 K using a volumetric adsorption system, and the results were analyzed by applying adsorption isotherm equations (Langmuir, Freundlich, and Sips) and energy distribution function. It was found that CO2 adsorption capacities were well correlated with the structural characteristics of chitosan and zeolite, and the ratio of elements [N/C, Al/(Si + Al)] formed on the surface of the composite. Moreover, the CO2/N2 adsorption selectivity was calculated under the mixture conditions of 15 V : 85 V, 50 V : 50 V, and 85 V : 15 V using the Langmuir equation and the ideal adsorption solution theory (IAST).