• Title/Summary/Keyword: energy dispersive X-ray spectroscopy

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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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Calcium annealing approach to control of surface groups and formation of oxide in Ti3C2Tx MXene

  • Jung-Min Oh;Su Bin Choi;Taeheon Kim;Jikwang Chae;Hyeonsu Lim;Jae-Won Lim;In-Seok Seo;Jong-Woong Kim
    • Advances in nano research
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    • v.15 no.1
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    • pp.1-13
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    • 2023
  • Ti3C2Tx MXene, a 2D material, is known to exhibit unique characteristics that are strongly dependent on surface termination groups. Here, we developed a novel annealing approach with Ca as a reducing agent to simultaneously remove F and O groups from the surface of multilayered MXene powder. Unlike H2 annealing that removes F effectively but has difficulty in removing O, annealing with Ca effectively removed both O and F. X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy revealed that the proposed approach effectively removed F and O from the MXene powder. The results of O/N analyses showed that the O concentration decreased by 57.5% (from 2.66 to 1.13 wt%). In addition, XPS fitting showed that the volume fraction of metal oxides (TiO2 and Al2O3) decreased, while surface termination groups (-O and -OH) were enhanced, which could increase the hydrophilic and adsorption properties of the MXene. These findings suggest that when F and O are removed from the MXene powder, the interlayer spacing of its lattice structure increases. The proposed treatment also resulted in an increase in the specific surface area (from 5.17 to 10.98 m2/g), with an increase in oxidation resistance temperature in air from ~436 to ~667 ℃. The benefits of this novel technology were verified by demonstrating the significantly improved cyclic charge-discharge characteristics of a lithium-ion battery with a Ca-treated MXene electrode.

A Simple and Quick Chemical Synthesis of Nanostructured Bi2Te3, Sb2Te3, and BixSb2-xTe3

  • Kim, Hee-Jin;Lee, Ki-Jung;Kim, Sung-Jin;Han, Mi-Kyung
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1123-1127
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    • 2010
  • We report a simple and quick route for the preparation of high-quality, nearly monodisperse $Bi_2Te_3$, $Sb_2Te_3$, and $Bi_xSb_{2-x}-Te_3$ nanocrystallites. The reactions of bismuth acetate or antimony acetate with Te in oleic acid result in pure phase of $Bi_2Te_3$ or $Sb_2Te_3$ nanoparticles, respectively. Also, ternary $Bi_xSb_{2-x}Te_3$ nanoparticles were successfully synthesized using the same method. The size and morphology of the nanoparticles were controlled by varying the stabilizing agents. The as-prepared nanoparticles are characterized by X-ray diffraction, scanning electron microscope, and high-resolution transmission electron microscope using an energy dispersive spectroscopy.

Synthesis of barium-doped PVC/Bi2WO6 composites for X-ray radiation shielding

  • Gholamzadeh, Leila;Sharghi, Hamed;Aminian, Mohsen Khajeh
    • Nuclear Engineering and Technology
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    • v.54 no.1
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    • pp.318-325
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    • 2022
  • In this study, composites containing undoped and barium-doped Bi2WO6:Ba2+were investigated for their shielding against diagnostic X-ray. At first, Bi2WO6 and barium-doped Bi2WO6 were synthesized with different weight percentages of barium oxide through a hydrothermal process. The as-synthesized nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and Raman spectroscopy (RS). After that, some shields were generated with undoped and barium-doped Bi2WO6:Ba2+ nanostructure particles incorporated into polyvinyl chloride (PVC) polymer with different thicknesses and 15% weight of the nanostructure. Finally, the prepared samples were exposed to an X-ray tube at 40, 80, and 120 kV voltages, 10 mAs and, 44.5 cm SID (i.e. the distance from the X-ray beam source to the specimen). Linear and mass attenuation coefficients were also calculated for different samples. The results indicated that, among the samples, the one with 7.5 mmol barium-doped Bi2WO6 had the most attenuation at the voltage of 40kV, and the attenuation coefficients would increase with an increase in the amount of barium. The samples with 15 and 17.5 mmol barium-doped Bi2WO6 had higher attenuation than the others at 80 and 120 kV. Moreover, the half-value layer (HVL), tenth-value layer (TVL) and 0.25 mm lead equivalent thickness were calculated for all the samples. The lowest HVL value was for the sample with 7.5 mmol barium-doped Bi2WO6. As the result clearly show, an increment in the barium-doping content leads to a decrease in both HVL and TVL. In every three voltages, 0.25 mm lead equivalent thickness of the barium-doped composites (7.5 mmol and 15 mmol) had less than the other composites. The lowest value of 0.25 mm lead equivalent thickness was 7.5 barium-doped in 40 kV voltage and 15 mmol barium-doped in 80 kV and 120 kV voltages. These results were obtained only for 15% weight of the nanostructure.

Evaluation of TiN-Zr Hydrogen Permeation Membrane by MLCA (Material Life Cycle Assessment) (물질전과정평가(MLCA)를 통한 TiN-Zr 수소분리막의 환경성 평가)

  • Kim, Min-Gyeom;Son, Jong-Tae;Hong, Tae-Whan
    • Clean Technology
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    • v.24 no.1
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    • pp.9-14
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    • 2018
  • In this study, Material life cycle evaluation was performed to analyze the environmental impact characteristics of TiN-Zr membrane manufacturing process. The software of MLCA was Gabi. Through this, environmental impact assessment was performed for each process. Transition metal nitrides have been researched extensively because of their properties. Among these, TiN has the most attention. TiN is a ceramic materials which possess the good combination of physical and chemical properties, such as high melting point, high hardness, and relatively low specific gravity, high wear resistance and high corrosion resistance. With these properties, TiN plays an important role in functional materials for application in separation hydrogen from fossil fuel. Precursor TiN was synthesized by sol-gel method and zirconium was coated by ball mill method. The metallurgical, physical and thermodynamic characteristics of the membranes were analyzed by using Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDS), X-ray Diffraction (XRD), Thermo Gravimetry/Differential Thermal Analysis (TG/DTA), Brunauer, Emmett, Teller (BET) and Gas Chromatograph System (GP). As a result of characterization and normalization, environmental impacts were 94% in MAETP (Marine Aquatic Ecotoxicity), 2% FAETP (Freshwater Aquatic Ecotoxicity), 2% HTP (Human Toxicity Potential). TiN fabrication process appears to have a direct or indirect impact on the human body. It is believed that the greatest impact that HTP can have on human is the carcinogenic properties. This shows that electricity use has a great influence on ecosystem impact. TiN-Zr was analyzed in Eco-Indicator '99 (EI99) and CML 2001 methodology.

Role of A phase Separating Element on the Plasticity of Amorphous Alloys : Experiment and Atomic Simulation Study (비정질 합금의 소성에 미치는 조성분리 원소의 역할 : 실험 및 전산모사 연구)

  • Park, Kyoung-Won;Lee, Chang-Myeon;Sa, In-Young;Lee, Byeong-Joo;Lee, Jae-Chul
    • Korean Journal of Materials Research
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    • v.19 no.2
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    • pp.79-84
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    • 2009
  • A series of experiments demonstrated that an addition of Ag into $(Cu_{0.5}Zr_{0.5})_{100-x}Ag_{x}$ amorphous alloys alters the plasticity of the alloys in a systematic manner. Energy dispersive x-ray spectroscopy (EDS) conducted on the $(Cu_{0.5}Zr_{0.5})_{100-x}Ag_{x}$ alloys exhibited the presence of compositional modulation, indicating that compositional separation had occurred. The presence of compositional modulation was also validated using a combined technique of molecular dynamics and Monte Carlo simulation. In this study, the effect of Ag on the compositional separation in $(Cu_{0.5}Zr_{0.5})_{100-x}Ag_{x}$ bulk amorphous alloys was investigated to understand the role played by the phase-separating element on the plasticity of the amorphous alloys.

Compositional and microstructural analyses of grayish-blue-powdered celadon in Yeongseo Region in Gangwon-do:by Wonju Beopcheon-temple site (강원도 영서지역 출토 분청사기의 조성 및 미세구조 분석: 원주(原州) 법천사지(法泉寺址)를 중심으로)

  • Lee, Byoung-Hoon;So, Myoung-Gi
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.211-221
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    • 2013
  • This research aims to examine compositional and microstructural properties of grayish-blue-powdered celadon in Wonju Beopcheon-temple site. X-ray fluorescence sequential spectroscopy (XRF) with micro-point analysis, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) were applied to determine the chemical composition, microstructure and crystallinity of samples, respectively. As a result, the average compositions of bodies were low silica ($RO_2$) and high flux (RO+$R_2O$). Owing to the high content of calcium oxide the glaze is considered lime type between limealkali type. The body of celdon sheard was found quarts, mullite, microcline, albite. Especially, the body's chemical compositions were compared to the results of previous studies by using a Seger formula. The compositional properties of Grayish-blue-powdered celadon in Wonju Beopcheon-temple site showed diffrently from the the other grayish-blue-powdered celadon.

Gas Sensing Properties of Powder Prepared from Waste Thermoelectric Devices by Wet Reduction Process

  • So, Hyeongsub;Im, Dong-Ha;Jung, Hyunsung;Lee, Kun-Jae
    • Journal of the Korean Ceramic Society
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    • v.55 no.1
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    • pp.90-93
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    • 2018
  • In this study, n-type $Bi_2Te_3$ in thermoelectric scrap is recovered through a wet reduction process. The recovered powder (tellurium) is grafted onto gas sensor in a new application that is not a thermoelectric device. Bismuth-rich powder is prepared by adding hydrazine when pH of the solution is brought to 13 using NaOH. The pH of the filtered solution was reduced using $HNO_3$, and then hydrazine was added to perform the re-reduction reaction. The tellurium-rich powder can be obtained through this reaction. The elemental analysis for these powders is confirmed by energy dispersive X-ray spectroscopy (EDS) analysis ; the successful separation of bismuth and tellurium is confirmed. Separated tellurium powder is mixed with DMF solvent and ethyl cellulose binder to confirm gas sensing properties. The tellurium paste was exposed in $NO_x$ atmosphere and exhibited a rapid reaction rate and recovery rate of less than 3 minutes for the gas.

Microscopical and chemical surface characterization of CAD/CAM zircona abutments after different cleaning procedures. A qualitative analysis

  • Gehrke, Peter;Tabellion, Astrid;Fischer, Carsten
    • The Journal of Advanced Prosthodontics
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    • v.7 no.2
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    • pp.151-159
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    • 2015
  • PURPOSE. To describe and characterize the surface topography and cleanliness of CAD/CAM manufactured zirconia abutments after steaming and ultrasonic cleaning. MATERIALS AND METHODS. A total of 12 ceramic CAD/CAM implant abutments of various manufacturers were produced and randomly divided into two groups of six samples each (control and test group). Four two-piece hybrid abutments and two one-piece abutments made of zirconium-dioxide were assessed per each group. In the control group, cleaning by steam was performed. The test group underwent an ultrasonic cleaning procedure with acetone, ethyl alcohol and antibacterial solution. Groups were subjected to scanning electron microscope (SEM) analysis and Energy-dispersive X-ray spectroscopy (EDX) to verify and characterize contaminant chemical characterization non- quantitatively. RESULTS. All zirconia CAD/CAM abutments in the present study displayed production-induced wear particles, debris as well as organic and inorganic contaminants. The abutments of the test group showed reduction of surface contamination after undergoing an ultrasonic cleaning procedure. However, an absolute removal of pollutants could not be achieved. CONCLUSION. The presence of debris on the transmucosal surface of CAD/CAM zirconia abutments of various manufacturers was confirmed. Within the limits of the study design, the results suggest that a defined ultrasonic cleaning process can be advantageously employed to reduce such debris, thus, supposedly enhancing soft tissue healing. Although the adverse long-term influence of abutment contamination on the biological stability of peri-implant tissues has been evidenced, a standardized and validated polishing and cleaning protocol still has to be implemented.

Preparation of Ni Nanoparticles-TiO2 Nanotube Arrays Composite and Its Application for Electrochemical Capacitor

  • He, Huichao;Zhang, Yunhuai;Xiao, Peng;Yang, Yannan;Lou, Qing;Yang, Fei
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1613-1616
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    • 2012
  • Ni nanoparticles-$TiO_2$ nanotube arrays (Ni/$TiO_2NTs$) composites were prepared by pulsed electrodeposition method and subsequently characterized by means of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX). The FESEM results showed that highly dispersed Ni nanoparticles were not only loaded on the top of the $TiO_2NTs$ but also within the tubular structure, and the particle size of Ni prepared at different current amplitude (100, 200 and 300 $mA{\cdot}cm^{-2}$) was in the range of 15 to 70 nm. The electrochemical studies indicated that Ni nanoparticles loaded on the highly ordered $TiO_2NTs$ are readily accessible for electrochemical reactions, which improve the efficiency of the Ni nanoparticles and $TiO_2NTs$. A maximum specific capacitance (27.3 $mF.cm^{-2}$) was obtained on the Ni/$TiO_2NTs$ composite electrode that prepared at a current of 200 $mA.cm^{-2}$, and the electrode also exhibited excellent electrochemical stability.