• Title/Summary/Keyword: XPS analysis

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Structural and Optical Properties of TiO2 Thin Films Prepared by RF Reactive Magnetron Sputtering (RF reactive magnetron sputtering으로 제조한 TiO2 박막의 구조 및 광학적 특성)

  • Gang, Gye-Won;Lee, Yeong-Hun;Gwak, Jae-Cheon;Lee, Dong-Gu;Jeong, Bong-Gyo;Park, Seong-Ho;Choe, Byeong-Ho
    • Korean Journal of Materials Research
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    • v.12 no.6
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    • pp.452-457
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    • 2002
  • Titanium oxide films were prepared by RF reactive magnetron sputtering. The effect of sputtering conditions on structural and optical properties was investigated systemically as a function of sputtering pressure(5~20 mTorr) and $O_2/Ar$ flow ratio(0.08~0.4). The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. At low sputtering pressure and $O_2/Ar$ flow ratio, the films had preferred orientations along [101] and [200] directions. As the sputtering pressure and $O_2/Ar$ flow ratio increased, the intensity of the 101 and 200 diffraction peaks decreased gradually. The microstructure of the sputtered films showed the fine grain size (20nm~50nm) and columnar microcrystals perpendicular to the substrate. With increasing the sputtering pressure and decreasing $O_2/Ar$ flow ratio, the sputtered films showed the more porous columnar structure. XPS analysis showed that stoichiometric $TiO_2$ films were deposited at 7 mTorr sputtering pressure and 0.2 $O_2/Ar$ flow ratio. The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. Ellipsometeric analysis showed that the refractive index increased from 2.32 to 2.46 as the sputtering pressure decreased. The packing density calculated using the refractive index varied from 0.923 to 0.976, indicating that $TiO_2$films became denser as the sputtering pressure decreased.

Improvement of Fouling Resistance with Reverse Osmosis Membrane Using Multi-layer Silane-Epoxy Surface Modification (실란-에폭시 다층 표면개질을 통한 역삼투막의 내오염성 향상)

  • Kwon, Sei;Lee, Yong Taek
    • Membrane Journal
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    • v.25 no.4
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    • pp.332-342
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    • 2015
  • In this study, to solve the major problem of reverse osmosis (RO) membrane, surface of reverse osmosis membrane was modified by silane-epoxy multi layer. Octyltrimethoxysilane (OcTES) was polymerized to membrane surface via cross-linking by Sol-gel method. n = 8 alkylgroup of OcTES formed the branch structure by self assembly. And for improve fouling resistance of RO membrane, Ether group of ethylene glycol diglycidyl ether (EGDE) was given to improve hydrophilicity of RO membrane surface by ring-opening. To analyze structure of RO membrane surface with FE-TEM and AFM. Membrane surface of the ridge and valley structure and the bridge structure was confirmed due to the multi-layer surface modification of OcTES and EGDE. And through the increase of the roughness, the branch structure was formed well on membrane surface. Through the XPS analysis was identified chemical structure of membrane surface. And confirmed that the hydrophilic surface modification is given to the surface of the film through a Contact angle analysis. In optimization of EGDE surface modification condition, was suitable 0.5 wt% EGDE concentraion and $70^{\circ}C$ ring-opening temperature. In result of fouling resistance test and MFI is SUL-H10, $PA-OcTES_{1.0}$, $PA-OcTES_{1.0}-EGDE_{0.5}$ 68.7, 60.4, 5.4 ($10E-8hr/mL^2$), multi-layer surface modified membrane improved fouling resistance.

Characterization of Nitrogen-Doped $TiO_2$ Thin Films Prepared by Metalorganic Chemical Vapor Deposition (유기금속 화학 기상증착법으로 실리콘 기판위에 증착된 질소치환 $TiO_2$ 박막의 특성분석)

  • 이동헌;조용수;이월인;이전국;정형진
    • Journal of the Korean Ceramic Society
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    • v.31 no.12
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    • pp.1577-1587
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    • 1994
  • TiO2 thin films with the substitution of oxygen with nitrogen were deposited on silicon substrate by metalorganic chemical vapor deposition (MOCVD) using Ti(OCH(CH3)2)4 (titanium tetraisopropoxide, TTIP) and N2O as source materials. X-ray diffraction (XRD) results indicated that the crystal structure of the deposited thin films was anatase TiO2 with only (101) plane observed at the deposition temperatures of 36$0^{\circ}C$ and 38$0^{\circ}C$, and with (101) and (200) plane at above 40$0^{\circ}C$. Raman spectroscopic results indicated that the crystal structure was anatase TiO2 in accordance with the XRD results without any rutile, fcc TiN, or hcp TiN structure. No fundamental difference was observed with temperature increase, but the peak intensity at 194.5 cm-1 increased with strong intensity at 143.0 cm-1 for all samples. The crystalline size of the films varied from 49.2 nm to 63.9 nm with increasing temperature as determined by slow-scan XRD experiments. The refractive index of the films increased from 2.40 to 2.55 as temperature increased. X-ray photoelectron spectroscopy (XPS) study showed only Ti 2s, Ti 2p, C 1s, O 1s and O 2s peaks at the surface of the film. The composition of the surface was estimated to be TiO1.98 from the quatitative analysis. In the bulk of the film Ti 2s, Ti 2p, O 1s, O 2s, N 1s and N 2s were detected, and Ti-N bonding was observed due to the substitution of oxygen with nitrogen. A satellite structure was observed in the Ti 2p due to the Ti-N bonding, and the composition of titanium nitride was determined to be about TiN1.0 from the position of the binding energy of Ti-N 2p3/2 and the quatitative analysis. The spectrum of Ti 2p energy level could be the sum of a 4, 5, or 6 Gaussian curve reconstruction, and the case of the sum of the 6 Gaussian curve reconstruction was physically most meaningful. From the results of Auger electron spectroscopy (AES), it was known that the composition was not varied significantly throughout the whole thickness of the film, and silicon oxide was not observed at the interface between the film and the substrate. The composition of the film was possible (TiO2)1-x.(TiN)x or TiO2-2xNx and in this experimental condition x was found to be about 0.21-0.16.

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Quantitative analysis of formation of oxide phases between SiO2 and InSb

  • Lee, Jae-Yel;Park, Se-Hun;Kim, Jung-Sub;Yang, Chang-Jae;Kim, Su-Jin;Seok, Chul-Kyun;Park, Jin-Sub;Yoon, Eui-Joon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.162-162
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    • 2010
  • InSb has received great attentions as a promising candidate for the active layer of infrared photodetectors due to the well matched band gap for the detection of $3{\sim}5\;{\mu}m$ infrared (IR) wavelength and high electron mobility (106 cm2/Vs at 77 K). In the fabrication of InSb photodetectors, passivation step to suppress dark currents is the key process and intensive studies were conducted to deposit the high quality passivation layers on InSb. Silicon dioxide (SiO2), silicon nitride (Si3N4) and anodic oxide have been investigated as passivation layers and SiO2 is generally used in recent InSb detector fabrication technology due to its better interface properties than other candidates. However, even in SiO2, indium oxide and antimony oxide formation at SiO2/InSb interface has been a critical problem and these oxides prevent the further improvement of interface properties. Also, the mechanisms for the formation of interface phases are still not fully understood. In this study, we report the quantitative analysis of indium and antimony oxide formation at SiO2/InSb interface during plasma enhanced chemical vapor deposition at various growth temperatures and subsequent heat treatments. 30 nm-thick SiO2 layers were deposited on InSb at 120, 160, 200, 240 and $300^{\circ}C$, and analyzed by X-ray photoelectron spectroscopy (XPS). With increasing deposition temperature, contents of indium and antimony oxides were also increased due to the enhanced diffusion. In addition, the sample deposited at $120^{\circ}C$ was annealed at $300^{\circ}C$ for 10 and 30 min and the contents of interfacial oxides were analyzed. Compared to as-grown samples, annealed sample showed lower contents of antimony oxide. This result implies that reduction process of antimony oxide to elemental antimony occurred at the interface more actively than as-grown samples.

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Improved Electrical Properties by In Situ Nitrogen Incorporation during Atomic Layer Deposition of HfO2 on Ge Substrate (Ge 기판 위에 HfO2 게이트 산화물의 원자층 증착 중 In Situ 질소 혼입에 의한 전기적 특성 변화)

  • Kim, Woo-Hee;Kim, Bum-Soo;Kim, Hyung-Jun
    • Journal of the Korean Vacuum Society
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    • v.19 no.1
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    • pp.14-21
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    • 2010
  • Ge is one of the attractive channel materials for the next generation high speed metal oxide semiconductor field effect transistors (MOSFETs) due to its higher carrier mobility than Si. But the absence of a chemically stable thermal oxide has been the main obstacle hindering the use of Ge channels in MOS devices. Especially, the fabrication of gate oxide on Ge with high quality interface is essential requirement. In this study, $HfO_xN_y$ thin films were prepared by plasma-enhanced atomic layer deposition on Ge substrate. The nitrogen was incorporated in situ during PE-ALD by using the mixture of nitrogen and oxygen plasma as a reactant. The effects of nitrogen to oxygen gas ratio were studied focusing on the improvements on the electrical and interface properties. When the nitrogen to oxygen gas flow ratio was 1, we obtained good quality with 10% EOT reduction. Additional analysis techniques including X-ray photoemission spectroscopy and high resolution transmission electron microscopy were used for chemical and microstructural analysis.

The Effects of Substrate Bias Voltage on the Formation of $(ZnS)_{1-x}-(SiO_2)_x$ Protective Films in Phase Change Optical Disk by R.F. Sputtering Method. (R.F. 스퍼터링법에 의한 상변화형 광디스크의 $(ZnS)_{1-x}-(SiO_2)_x$ 보호막 제조시 기판 바이어스전압의 영향)

  • Lee, Tae-Yun;Kim, Do-Hun
    • Korean Journal of Materials Research
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    • v.8 no.10
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    • pp.961-968
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    • 1998
  • In order to investigate the effects of substrate bias voltage on the formation of$ZnS-SiO_2$ protective film in phase change optical disk by R.F. magnetron sputtering method, thin dielectric film was formed on Si wafer and Corning glass by using ZnS(80mol%)-$SiO_2$(20mol%)t arget under argon gas. In this study, the Taguchi experimental method was applied in order to obtain optimum conditions with reduced number of experiments and to control numerous variables effectively. At the same time this method can assure the reproducibility of experiments. Optimum conditions for film formation obtained by above method were target RF power of 200 W. substrate RF power of 20 W, Ar pressure of 5 mTorr. sputtering time of 20 min.. respectively. The phase of specimen was determined by using XRD and TEM. The compositional analysis of specimen was performed by XPS test. In order to measure the thermal resistivity of deposited specimen, annealing test was carried out at $300^{\circ}C$ and $600^{\circ}C$. For the account of void fraction in thin film, the Bruggeman EMA(Effective Medium Approximation) method was applied using the optical data obtained by Spectroscopic Ellipsometry. According to the results of this work, the existence of strong interaction between bias voltage and sputtering time was confirmed for refractive index value. According to XRD and TEM analysis of specimen, the film structure formed in bias voltage resulted in more refined structures than that formed without bias voltage. But excess bias voltage resulted in grain growth in thin film. It was confirmed that the application of optimum bias voltage increased film density by reduction of void fraction of about 3.7%.

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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).

The surface kinetic properties of $ZrO_2$ Thin Films in dry etching by Inductively Coupled Plasma

  • Yang-Xue, Yang-Xue;Kim, Hwan-Jun;Kim, Dong-Pyo;Um, Doo-Seung;Woo, Jong-Chang;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.105-105
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    • 2009
  • $ZrO_2$ is one of the most attractive high dielectric constant (high-k) materials. As integrated circuit device dimensions continue to be scaled down, high-k materials have been studied more to resolve the problems for replacing the EY31conventional $SiO_2$. $ZrO_2$ has many favorable properties as a high dielectric constant (k= 20~25), wide band gap (5~7 eV) as well as a close thermal expansion coefficient with Si that results in good thermal stability of the $ZrO_2/Si$ structure. In order to get fine-line patterns, plasma etching has been studied more in the fabrication of ultra large-scale integrated circuits. The relation between the etch characteristics of high-k dielectric materials and plasma properties is required to be studied more to match standard processing procedure with low damaged removal process. Due to the easy control of ion energy and flux, low ownership and simple structure of the inductively coupled plasma (ICP), we chose it for high-density plasma in our study. And the $BCl_3$ included in the gas due to the effective extraction of oxygen in the form of $BCl_xO_y$ compound In this study, the surface kinetic properties of $ZrO_2$ thin film was investigated in function of Ch addition to $BCl_3/Ar$ gas mixture ratio, RF power and DC-bias power based on substrate temperature. The figure 1 showed the etch rate of $ZrO_2$ thin film as function of gas mixing ratio of $Cl_2/BCl_3/Ar$ dependent on temperature. The chemical state of film was investigated using x-ray photoelectron spectroscopy (XPS). The characteristics of the plasma were estimated using optical emission spectroscopy (OES). Auger electron spectroscopy (AES) was used for elemental analysis of etched surface.

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Effect of Support Geometry on Catalytic Activity of Pt/CeO2 Nanorods in Water Gas Shift Reaction (Water Gas Shift 반응에서 Pt/CeO2 촉매의 지지체구조에 따른 촉매활성 연구)

  • Im, Hyo Been;Kwon, Soon Jin;Byun, Chang Ki;Ahn, Hee Sung;Koo, Kee Young;Yoon, Wang Lai;Yi, Kwang Bok
    • Journal of Hydrogen and New Energy
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    • v.25 no.6
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    • pp.577-585
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    • 2014
  • Nanorod and particle shape $CeO_2$ were synthesized via hydrothermal process and precipitation method, respectively, and used as supports of Pt catalyst for water gas shift (WGS) reaction. Three different durations (12, 48, and 96h) for hydrothermal process were applied for the preparation of nanorod type $CeO_2$. 1.0 wt% of Pt was loaded on the prepared supports with incipient wetness method prior to the catalytic activity tests that were carried out at a GHSV of $95,541h^{-1}$, and a temperature range of 200 to $360^{\circ}C$. Varying duration of hydrothermal process led to the difference in physical characteristics of $CeO_2$ nanorods, such as aspect ratio, BET surface area, pore diameter, and pore volume. Consequently, the catalytic activities of Pt/$CeO_2$ nanorods were affected by the physical characteristics of the supports and appeared to be in the order of Pt/$CeO_2$(12) > Pt/$CeO_2$(48) > Pt/$CeO_2$(96). The comparison of the catalytic activities and results of the analysis (XPS, XRD, SEM, BET and TPR) for the supports revealed that the activity of the catalysts depends on chemical states of the Pt and the support materials in the temperature range that is lower than $280^{\circ}C$. However, the activity is rather dependent on the physical characteristic of the supports because the increased gas velocity limits the mass transfer of reactants in micropores of the supports.

Preparation and Characterization of PVA/PSSA-MA Electrolyte Membranes Containing Silica Compounds and Surface Fluorination for Fuel Cell Applications (연료전지 응용을 위한 실리카 성분을 함유하며 표면불소화된 PVA/PSSA-MA 막의 제조 및 특성 연구)

  • Kim, Dae-Hoon;Lee, Bo-Sung;Rhim, Ji-Won
    • Polymer(Korea)
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    • v.34 no.6
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    • pp.540-546
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    • 2010
  • In this manuscript, in order to reduce methanol permeability and, at the same time, to increase proton conductivity THS-PSA containing silica compound, responsible for methanol permeability reduction, and sulfonic acid, responsible for proton conductivity enhancement, was applied onto PVA/PSSA-MA membranes. And in order to improve durability, the resulting membranes, PVA/PSSAMA/THS-PSA, were exposed to 500ppm F2 gas at varying reaction times. The surface-fluorinated membranes were characterized through the measurement of contact angles, thermo-gravimetric analysis, and X-ray photoelectron spectroscopy to observe the physico-chemical changes. For the evaluation of the electro-chemical changes in the resulting membranes, its water contents, ion exchange capacity, proton conductivity, and methanol permeability were measured and then compared with the commercial membrane, Nafion 115. Finally, the membran electrode assembly(MEA) was prepared and the cell voltage against the current density was measured. As fluorination time increased, the contents of F2 increased up to maximum 4.3% and to depth of 50 nm. At 60 min of fluorination, the proton conductivity was 0.036 S/cm, larger than Nafion 115 at 0.024 S/cm, and the methanol permeability was $9.26E-08cm^2/s$, less than Nafion 115 at $1.17E-06cm^2/s$.