• Title/Summary/Keyword: Electron energy loss spectroscopy

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Understanding the Viscoelastic Properties and Surface Characterization of woodflour-Polypropylene Composites (목분-폴리프로필렌 복합재의 점탄성적 성질과 표면특성)

  • Son, Jungil;Gardner, Douglas J.
    • Journal of Adhesion and Interface
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    • v.3 no.4
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    • pp.1-9
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    • 2002
  • The main goal of this study was to analyze the effect of process additives, i.e. maleated polypropylene (MAPP), and nucleating agent on the viscoelastic properties of different types of extruded polypropylene-wood plastic composites manufactured from either PP homopolymer, high crystallinity PP or PP impact copolymer using dynamic mechanical thermal analysis. And also, the esterification reaction between wood flour and maleated polypropylene, and its role in determining the mechanical properties of wood flour-polypropylene composites was investigated. The wood plastic composites were manufactured using 60% pine wood flour and 40% polypropylene on a Davis-Standard $Woodtruder^{TM}$. Dynamic mechanical thermal properties, polymer damping peaks(than ${\delta}$), storage modulus (E') and loss modulus (E") were measured using a dynamic mechanical thermal analyzer. XPS (X-ray Photoelectron Spectroscopy), also known as ESCA (Electron Spectroscopy for Chemical Analysis) study of wood flour treated with MAPP was performed to obtain information on the chemical nature of wood fiber before and after treatment. To analyze the effect of frequency on the dynamic mechanical properties of the various composites, DMA tests were performed over a temperature range of -20 to $100^{\circ}C$, at four different frequencies (1, 5, 10 and 25 Hz), and at a heating rate of $5^{\circ}C/min$. From these results, the activation energy of the various composite was measured using an Arrhenius relationship to investigate the effect of maleated PP and nucleating agent on the measurement of the interphase between the wood and plastic of the extruded polypropylene wood plastic composites.

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Corrosion Inhibition Studies on Low Carbon Steel in Hydrochloric Acid Medium Using o-Vanillin-Glutamine Schiff Base

  • Thusnavis, G. Rexin;Archana, T.V.;Palanisamy, P.
    • Corrosion Science and Technology
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    • v.21 no.1
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    • pp.32-40
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    • 2022
  • The o-Vanillin - Glutamine Schiff base [2-Hydroxy-3-Methoxy BenzylidineCarbomyl) -2-Butanoic Acid] was examined for low carbon steel corrosion inhibition in acid media. Weight loss studies were carried out at three different temperatures to determine the inhibition efficiency (IE). Electrochemical impedance spectroscopy revealed that the charge transfer resistance controlled the corrosion reaction and Tafel polarization indicated that the Schiff base acts as mixed mode of inhibitor. SEM images were recorded for the surface morphology of the low carbon steel surface. DFT studies revealed corrosion control mechanisms using quantum chemical parameters such as EHOMO, ELUMO, energy gap (∆E), chemical Hardness (η), chemical Softness (σ), Electronegativity (χ), and the fraction of electron transferred (∆N), which is calculated using Gaussian software 09. The gas-phase geometry was fully optimized in the Density Functional Theory (DFT/B3LYP-6-31G (d)).The DFT results are in good agreement with the experimental results. All the results proved that the Schiff Base (2-Hydroxy-3-Metoxy BenzylidineCarbomyl) -2-Butanoic is a suitable alternative for corrosion inhibition of low carbon steel in acid media.

Atomic layer chemical vapor deposition of Zr $O_2$-based dielectric films: Nanostructure and nanochemistry

  • Dey, S.K.
    • Electrical & Electronic Materials
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    • v.16 no.9
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    • pp.64.2-65
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    • 2003
  • A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{+}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{+}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.

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Variation in the Nanostructural Features of the nc-Si:H Thin Films with Substrate Temperature (수소화된 나노결정 실리콘 박막의 기판온도에 따른 나노구조 변화)

  • Nam, Hee-Jong;Son, Jong-Ick;Cho, Nam-Hee
    • Korean Journal of Materials Research
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    • v.23 no.7
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    • pp.359-365
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    • 2013
  • We investigated the nanostructural, chemical and optical properties of nc-Si:H films according to deposition conditions. Plasma enhanced chemical vapor deposition(PECVD) techniques were used to produce nc-Si:H thin films. The hydrogen dilution ratio in the precursors, [$SiH_4/H_2$], was fixed at 0.03; the substrate temperature was varied from room temperature to $600^{\circ}C$. By raising the substrates temperature up to $400^{\circ}C$, the nanocrystalite size was increased from ~2 to ~7 nm and the Si crystal volume fraction was varied from ~9 to ~45% to reach their maximum values. In high-resolution transmission electron microscopy(HRTEM) images, Si nanocrystallites were observed and the crystallite size appeared to correspond to the crystal size values obtained by X-ray diffraction(XRD) and Raman Spectroscopy. The intensity of high-resolution electron energy loss spectroscopy(EELS) peaks at ~99.9 eV(Si $L_{2,3}$ edge) was sensitively varied depending on the formation of Si nanocrystallites in the films. With increasing substrate temperatures, from room temperature to $600^{\circ}C$, the optical band gap of the nc-Si:H films was decreased from 2.4 to 1.9 eV, and the relative fraction of Si-H bonds in the films was increased from 19.9 to 32.9%. The variation in the nanostructural as well as chemical features of the films with substrate temperature appears to be well related to the results of the differential scanning calorimeter measurements, in which heat-absorption started at a substrate temperature of $180^{\circ}C$ and the maximum peak was observed at ${\sim}370^{\circ}C$.

Mechanical Properties of Styrene-Butadiene Rubber Reinforced with Hybrids of Chitosan and Bamboo Charcoal/Silica

  • Li, Xiang Xu;Cho, Ur Ryong
    • Elastomers and Composites
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    • v.54 no.1
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    • pp.22-29
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    • 2019
  • Chitosan-polyvinyl alcohol (PVA) -bamboo charcoal/silica (CS-PVA-BC/SI) hybrid fillers with compatibilized styrene-butadiene rubber (SBR) composites were fabricated by the interpenetrating polymer network (IPN) method. The structure and composition of the composite samples were characterized by scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR). The viscoelastic behaviors of the rubber composites and their vulcanizates were explored using a rubber processing analyzer (RPA) in the rheometer, strain sweep and temperature sweep modes. The storage and loss moduli of SBR increased significantly with the incorporation of different hybrid fillers, which was attributed to the formation of an interphase between the hybrid fillers and rubber matrix, and the effective dispersion of the hybrid fillers. The mechanical properties (hardness, tensile strength, oxygen transmission rate, and swelling rate) of the composite samples were characterized in detail. From the results of the mechanical test, it was found that BC-CS-PVA0SBR had the best mechanical properties. Therefore, the BC-CS-PVA hybrid filler provided the best reinforcement effects for the SBR latex in this research.

Dielectric and Optical Properties of Amorphous Hafnium Indium Zinc Oxide Thin Films on Glass Substrates

  • Shin, Hye-Chung;Seo, Soon-Joo;Denny, Yus Rama;Lee, Kang-Il;Lee, Sun-Young;Oh, Suhk-Kun;Kang, Hee-Jae;Heo, Sung;Chung, Jae-Gwan;Lee, Jae-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.225-225
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    • 2011
  • The dielectric and optical properties of GaInZnO (GIZO), HfInZnO (HIZO) and InZnO (IZO) thin films on glass by RF magnetron sputtering method were investiged using reflection electron energy loss spectroscopy (REELS). The band gap was estimated from the onset values of REELS spectra. The band gaps of GIZO, HIZO and IZO thin films are 3.1 eV, 3.5 eV and 3.0 eV, respectively, Hf and Ga incorporated into IZO results in an increase in the energy band gap of IZO by 0.5 eV and 0.1 eV. The dielectric functions were determined by comparing the effective cross section determined from experimental REELS with a rigorous model calculation based on the dielectric response theory, using available software package, good agreement between the experimental and fitting results gives confidence in the accuracy of the determined dielectric function. The main peak of Energy Loss Function (ELF) obtained from IZO shows at 18.42 eV, which shifted to 19.43 eV and 18.15 eV for GIZO and HIZO respectively, because indicates the corporation of cation Ga and Hf in the composition. The optical properties represented by the dielectric function e, the refractive index n, the extinction coefficient k, and the transmission coefficient, T of HIZO and IZO thin films were determined from a quantitative analysis of REELS. The transmission coefficient was increased to 93% and decreased to 87% in the visible region with the incorporation of Hf and Ga in the IZO compound.

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Preparation of ultra-clean hydrogen and deuterium terminated Si(111)-($1{\times}1$) surfaces and re-observation of the surface phonon dispersion curves

  • Kato, H.;Taoka, T.;Murugan, P.;Kawazoe, Y.;Yamada, T.;Kasuya, A.;Suto, S.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.4-5
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    • 2010
  • The surface phonon is defined as a coherent vibrational excitation of surface atoms propagating along the surface. It is characterized by a phonon dispersion curves, which were extensively studied in 1990's using helium atom scattering and high-resolution electron-energy-loss spectroscopy (HREELS)[1].The understanding is mainly based on the theoretical framework of a classical bond model or cluster calculations. The recent sample preparation and first principles calculations open the naval way to deep insight for surface phonon problems. The surface phonon dispersion on the hydrogen-terminated Si(111)-($1{\times}1$) surface [H:Si(111)] is the typical system and already reported experimentally [2] and theoretically [3], although the understandingis incomplete. The sample contaminated by the oxygen atoms on the surface and the calculations were also classical. In this study, firstly, we have prepared an ultra-clean H:Si(111) surface [4] and measured the surface phonon dispersion curvesusing HREELS. Secondly, we have performed first-principles density functional calculations with the projector augmented wave functionals, as implemented in VASP, using generalized gradient approximations. We used aslab of six silicon layers and both top and bottom surfaces were terminated with hydrogen atoms. Finally, we have compared with the surface phonon dispersion of deuterium-terminatedSi(111)-($1{\times}1$) surface[5] and led to our conclusions. The Si-H stretching and the bending modes are observed at 258.5 and 78.2 meV, respectively. These energies are the same as the previously reported values [2], but the energy-loss peaks at the lower energy regions are dramatically shifted. Through this combination study, we have formulated the procedure of preparing ultra-clean H:Si(111)/D:Si(111), which was confirmed by HREELS vibrational analysis. The Si surface will be utilized for further nano-physics research as well as for the materials for nano-fubrication.

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Effect of oxygen deficiency on electronic properties and local structure of amorphous tantalum oxide thin films

  • Denny, Yus Rama;Firmansyah, Teguh;Park, Chanae;Kang, Hee Jae;Yang, Dong-Seok;Heo, Sung;Chung, Jae Gwan;Lee, Jae Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.122.1-122.1
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    • 2015
  • The dependence of electronic properties and local structure of tantalum oxide thin film on oxygen deficiency have been investigated by means of X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), and X-ray absorption spectroscopy (XAS). The XPS results showed that the oxygen flow rate change results in the appearance of features in the Ta 4f at the binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV whose peaks are attributed to Ta1+, Ta2+, Ta3+, Ta4+, and Ta5+, respectively. The presence of nonstoichiometric state from tantalum oxide (TaOx) thin films could be generated by the oxygen vacancies. The REELS spectra suggested the decrease of band gap for tantalum oxide thin films with increasing oxygen deficiency. In addition, XAS spectra manifested both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the decrease of oxygen deficiency.

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The Effect of the Oxygen Flow Rate on the Electronic Properties and the Local Structure of Amorphous Tantalum Oxide Thin Films

  • Denny, Yus Rama;Lee, Sunyoung;Lee, Kangil;Kang, Hee Jae;Yang, Dong-Seok;Heo, Sung;Chung, Jae Gwan;Lee, Jae Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.398-398
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    • 2013
  • The electronic properties and the local structure of tantalum oxide thin film with variation of oxygen flow rate ranging from 9.5 to 16 sccm (standard cubic centimeters per minute) have been investigated by X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), and X-ray absorption spectroscopy (XAS). The XPS results show that the Ta4f spectrum for all films consist of the strong spin-orbit doublet $Ta4f_{7/2}$ and $Ta4f_{5/2}$ with splitting of 1.9 eV. The oxygen flow rate of the film results in the appearance of new features in the Ta4f at binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV, these peaks attribute to $Ta^{1+}$, $Ta^{2+}$, $Ta^{4+}$/$Ta^{2+}$, and $Ta^{5+}$, respectively. Thus, the presence of non-stoichiometric state from tantalum oxide ($TaO_x$) thin films could be generated by the oxygen vacancies. The REELS spectra suggest the decrease of band gap for tantalum oxide thin films with increasing the oxygen flow rate. The absorption coefficient ${\mu}$ and its fine structure were extracted from the fluorescence mode of extended X-ray absorption fine structure (EXAFS) spectra. In addition, bond distances (r), coordination numbers (N) and Debye-Waller factors (${\sigma}^2$) each film were determined by a detailed of EXAFS data analysis. EXAFS spectrapresent both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the increase of oxygen flow rate.

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Crystallographic and Interfacial Characterization of Al2O3 and ZrO2 Dielectric Films Prepared by Atomic Layer Chemical Vapor Deposition on the Si Substrate (Si 기판에서 원자층 화학 기상 증착법으로 제조된 Al2O3 및 ZrO2 유전 박막의 결정학적 특성 및 계면 구조 평가)

  • Kim, Joong-Jung;Yang, Jun-Mo;Lim, Kwan-Yong;Cho, Heung-Jae;Kim, Won;Park, Ju-Chul;Lee, Soun-Young;Kim, Jeong-Sun;Kim, Geun-Hong;Park, Dae-Gyu
    • Korean Journal of Materials Research
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    • v.13 no.8
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    • pp.497-502
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    • 2003
  • Crystallographic characteristics and interfacial structures of $Al_2$$O_3$and $ZrO_2$dielectric films prepared by atomic layer chemical vapor deposition (ALCVD) were investigated at atomic scale by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDS)/electron energy-loss spectroscopy (EELS) coupled with a field-emission transmission electron microscope. The results obtained from cross-sectional and plan-view specimens showed that the $Al_2$$O_3$film was crystallized by annealing at a high temperature and its crystal system might be evaluated as either cubic or tetragonal phase. Whereas the $ZrO_2$film crystallized during deposition at a low temperature of ∼$300^{\circ}C$ was composed of both tetragonal and monoclinic phase. The interfacial thickness in both films was increased with the increased annealing temperature. Further, the interfacial structures of X$ZrO_2$$O_3$and $ZrO_2$films were discussed through analyses of EDS elemental maps and EELS spectra obtained from the annealed films, respectively.