• 제목/요약/키워드: energy dispersive X-ray spectroscopy

검색결과 639건 처리시간 0.03초

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

  • Dey, S.K.
    • E2M - 전기 전자와 첨단 소재
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    • 제16권9호
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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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    • 제15권1호
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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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    • 제31권5호
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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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    • 제54권1호
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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.

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

  • 김민겸;손종태;홍태환
    • 청정기술
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    • 제24권1호
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    • pp.9-14
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    • 2018
  • 본 연구에서는 TiN-Zr 수소분리막의 제조 공정에 대한 환경 영향 특성을 분석하기 위해 물질전과정평가를 수행하였다. Material Life Cycle Assessment (MLCA)의 소프트웨어로는 Gabi를 사용하였다. 이를 통하여 각 공정에서 미치는 영향과 특성화 별 환경영향평가를 수행하였다. 졸겔법에 의해 전구체 TiN을 합성하고 볼밀법을 이용하여 지르코늄을 코팅하였다. 이를 CIP, HPS에 의해 디스크 형으로 제작하였고 주사전자현미경(scanning electron microscopy, SEM), 에너지분산형 분광분석법(energy dispersive X-ray spectroscopy, EDS), X-선 회절분석기(X-ray diffraction, XRD), 열중량분석(thermo gravimetry/differential thermal analysis, TG/DTA), 비표면적분석(Brunauer, Emmett, Teller, BET) 및 가스 크로마토그래프 시스템(gas chromatograph system, GP)을 이용하여 분리막의 야금학적, 물리학적, 열역학적 특성을 분석하였다. 또한, 물질전과정평가를 위해 수행한 특성화와 정규화 결과, 영향범주 별 환경영향은 해양 생태 독성이 94%, 수계 생태 독성 2%, 인간독성 2%의 기여도를 보였다. 아울러, 제조공정 중 전기 사용이 생태계 영향에 큰 영향을 미친다는 것을 알 수 있었다. 물질 전 과정 평가는 Eco-Indicator '99 (EI99)와 CML 2001 방법론을 기반으로 분석하였다.

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

  • 박경원;이창면;사인영;이병주;이재철
    • 한국재료학회지
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    • 제19권2호
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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.

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

  • 이병훈;소명기
    • 분석과학
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    • 제26권3호
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    • pp.211-221
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    • 2013
  • 본 연구는 원주 법천사지에서 출토된 분청사기의 화학조성과 미세조직, 결정상을 X-선형광분석기와 주사전자현미경-에너지분산형엑스선분석기, X-선회절분석기를 이용하여 알아보았다. 태토의 화학성분 분석 결과, 낮은 실리카($RO_2$) 함량과 높은 융제(RO+$R_2O$) 함량임을 알 수 있다. 유약의 경우 융제 성분 중 CaO 함량이 높은 전형적인 석회계열(lime type)과 석회-알칼리 계열(lime-alkali type) 유약을 사용하였으며 태토의 결정상으로는 quarts, mullite, microcline, albite가 확인되었다. 특히 원주 법천사지에서 출토된 분청사기 태토의 화학적 조성은 제겔식을 이용하여 이미 연구된 다른 유적에서 출토된 분청사기와 비교하였으며 화학조성은 서로 상이한 결과를 보였다.

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

  • So, Hyeongsub;Im, Dong-Ha;Jung, Hyunsung;Lee, Kun-Jae
    • 한국세라믹학회지
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    • 제55권1호
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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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    • 제7권2호
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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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    • 제33권5호
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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.