• Title/Summary/Keyword: In-situ XRD

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Mechanical Behavior of Directionally Solicified (Y2O3)ZrO2/Al2O3 Eurtctic Fibers

  • Park, Deok-Yong;Yang, Jenn-Ming
    • Journal of the Korean Ceramic Society
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    • v.41 no.1
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    • pp.1-8
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    • 2004
  • The microstructural features and mechanical behavior of directionally solidified $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fibers after extended beat treatment in oxidizing environment were investigated. The fiber was grown continuously by an Edge-defined Film-fed Growth (EFG) technique. The microstructure was characterized using X-Ray Diffraction (XRD) and Scanning Electron Microscopy(SEM). The microstructure of the fiber in the as-fabricated state consists of highly oriented colonv and fine lamellar microstructure along the fiber axis. Tensile strength of the $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber remained unchanged with heat treatment at temperatures between $1200^{\circ}C$ and $1500^{\circ}C$ up to 300h. The weibulls modulus remained fairly constant after extended thermal exposure. The fracture toughness and crack propagation behavior were investigated. The fracture toughness ($K_{1C}$) of the $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber in the as-fabricated state were measured to be 3.6 ${\pm}$ 0.5 MPa${\cdot}m^{1/2}$ by an indentation technique and 2.2 ${\pm}$ 0.2 MPa${\cdot}m^{1/2}$ by assuming elliptical flaw of a semi-infinite solid, respectively. The $(Y_2O_3)ZrO_2/Al_2O_3$ eutectic fiber showed a radial (Palmqvist) crack type and exhibited an orthotropic crack growth behavior under 100 g load.

Template Synthesis and Characterization of Host (Nanocavity of Zeolite Y)-Guest ([Cu([18]aneN4S2)]2+, [Cu([20]aneN4S2)]2+, [Cu(Bzo2[18]aneN4S2)]2+, [Cu(Bzo2[20]aneN4S2)]2+) Nanocomposite Materials

  • Salavati-Niasari, Masoud;Mirsattari, Seyed Nezamodin;Saberyan, Kamal
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.348-354
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    • 2009
  • Copper(II) complexes with tetraoxo dithia tetraaza macrocyclic ligands; [18]ane$N_4S_2$: 1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, [20]ane$N_4S_2$: 1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane,Bzo2[18]ane$N_4S_2$: dibenzo-1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, Bzo2[20]ane$N_4S_2$: dibenzo-1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane; were entrapped in the nanopores of zeolite-Y by a two-step process in the liquid phase: (i) adsorption of [bis(diamine)copper(II)] (diamine = 1,2-diaminoethane, 1,3-diaminopropane, 1,2-diaminobenzene, 1,3-diaminobenzene); $[Cu(N-N)_2]^{2+}$-NaY; in the nanopores of the zeolite, and (ii) in situ template condensation of the copper(II) precursor complex with thiodiglycolic acid. The obtained complexes and new host-guest nanocomposite materials; $[Cu([18]aneN_4S_2)]^{2+}-NaY,\;[Cu([20]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[18]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[20]aneN_4S_2)]^{2+}$-NaY; have been characterized by elemental analysis FT-IR, DRS and UV-Vis spectroscopic techniques, molar conductance and magnetic moment data, XRD and, as well as nitrogen adsorption. Analysis of data indicates all of the complexes have been encapsulated within nanopore of zeolite Y without affecting the zeolite framework structure.

In Situ-DRIFTS Study of Rh Promoted CuCo/Al2O3 for Ethanol Synthesis via CO Hydrogenation

  • Li, Fang;Ma, Hongfang;Zhang, Haitao;Ying, Weiyong;Fang, Dingye
    • Bulletin of the Korean Chemical Society
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    • v.35 no.9
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    • pp.2726-2732
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    • 2014
  • The promoting effect of rhodium on the structure and activity of the supported Cu-Co based catalysts for CO hydrogenation was investigated in detail. The samples were characterized by DRIFTS, $N_2$-adsorption, XRD, $H_2$-TPR, $H_2$-TPD and XPS. The results indicated that the introduction of rhodium to Cu-Co catalysts resulted in modification of metal dispersion, reducibility and crystal structure. DRIFTS results of CO hydrogenation at reaction condition (P=2 MPa, $T=260^{\circ}C$) indicated the addition of 1 wt % rhodium improved hydrogenation ability of Cu-Co catalysts. The ethanol selectivity and CO conversion were both improved by 1 wt % Rh promoted Cu-Co based catalysts. The alcohol distribution over un-promoted and rhodium promoted Cu-Co based catalysts obeys A-S-F rule and higher chain growth probability was got on rhodium promoted catalyst.

Effect of CeO$_2$ buffer layer on the crystallization of YBCO thin film on Hastelloy substrate (비정질 금속 기판상에 증착된 YBCO 박막의 결정성에 대한 CEO$_2$ 완충막의 효과)

  • Kim, Sung-Min;Lee, Sang-Yeol
    • 한국초전도학회:학술대회논문집
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    • v.9
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    • pp.392-396
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    • 1999
  • Superconducting YBa$_2Cu_3O_{7-{\delta}}$(YBCO) thin films were grown on Hastelloy(Ni-Cr-Mo alloys) with CeO$_2$ buffer layer in-situ by pulsed laser deposition in a multi-target processing chamber. To apply superconducting property on power transmission line, we have deposited YBCO thin film on flexible metallic substrate. However, it is difficult to grow the YBCO films on flexible metallic substrates due to both interdiffusion problem between metallic substrate and superconducting overlayers and non-crystallization of YBCO on amorphous substrate. It is necessary to use a buffer layer to overcome the difficulties. We have chosen CeO$_2$ as a buffer layer which has cubic structure of 5.41 ${\AA}$ lattice parameter and only 0.2% of lattice mismatch with 3.82 ${\AA}$ of a-axis lattice parameter of YBCO on [110] direction of CeO$_2$ In order to enhance the crystallization of YBCO films on metallic substrates, we deposited CeO$_2$ buffer layers with varying temperature and 02 pressure. By XRD, it is observed that dominated film orientation is strongly depending on the deposition temperature of CeO$_2$ layer. The dominated orientation of CeO$_2$ buffer layer is changed from (200) to(111) by increasing the deposition temperature and this transition affects the crystallization of YBCO superconducting film on CeO$_2$ buffered Hastelloy.

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Effect of Pressure on Properties of the SiC-$TiB_2$ Electroconductive Ceramic Composites (SiC-$TiB_2$ 전도성(電導性) 복합체(複合體)의 특성(特性)에 미치는 가압(加壓)의 영향(影響))

  • Shin, Yong-Deok;Seo, Je-Ho;Ju, Jin-Young;Ko, Tae-Hun;Lee, Jung-Hoon
    • Proceedings of the KIEE Conference
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    • 2008.07a
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    • pp.1228-1229
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    • 2008
  • The composites were fabricated 61[vol.%] ${\beta}$-SiC and 39[vol.%] $TiB_2$ powders with the liquid forming additives of 12[wt%] $Al_2O_3+Y_2O_3$ as a sintering aid by pressure or pressureless annealing at 1,650[$^{\circ}C$] for 4 hours. Reactions between SiC and transition metal $TiB_2$ were not observed in the microstructure and the phase analysis of the SiC-$TiB_2$ electroconductive ceramic composites. Phase analysis of SiC-$TiB_2$ composites by XRD revealed mostly of ${\alpha}$-SiC(6H), $TiB_2$, and In Situ $YAG(Al_5Y_3O_{12})$. The relative density, the flexural strength and the Young's modulus showed the highest value of 88.32[%], 136.43[MPa] and 52.82[GPa] for pressure annealed SiC-$TiB_2$ composites at room temperature. The electrical resistivity showed the lowest value of 0.0162[${\Omega}{\cdot}cm$] for pressure annealed SiC-$TiB_2$ composite at 25[$^{\circ}C$]. The electrical resistivity of the pressure annealed SiC-$TiB_2$ composite was positive temperature coefficient resistance (PTCR) but the electrical resistivity of the pressureless annealed SiC-$TiB_2$ composites was negative temperature coefficient resistance(NTCR) in the temperature ranges from 25[$^{\circ}C$] to 700[$^{\circ}C$].

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The Role of (111)MgO Underlayer in Growth of c-axis Oriented Barium Ferrite Films

  • Erickson, D.W.;Hong, Y.K.;Gee, S.H.;Tanaka, T.;Park, M.H.;Nam, I.T.
    • Journal of Magnetics
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    • v.9 no.4
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    • pp.116-120
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    • 2004
  • Hexagonal barium-ferrite ($BaFe_{12}O_{19}$, magnetoplumbite structure; BaM) film with perpendicularly c-axis orientation was successfully deposited on (100) silicon substrates with an MgO (111) underlayer by rf diode sputtering and in-situ heating at $920^{\circ}C$. The magnetic and structural properties of 0.27 ${\mu}m$ thick BaM films on MgO (111) underlayers were compared to films of the same thickness deposited onto single-crystal MgO (111) and c-plane ($000{\ell}$) sapphire ($Al_2O_3$) substrates by vibrating sample magnetometry (VSM), x-ray diffractometer (XRD), and atomic force microscopy (AFM). The thickness dependence of MgO (111) underlayers on silicon wafer was found to have a large effect on both magnetic and structural properties of the BaM film. The thickness of 15 nm MgO (111) underlayers produced BaM films with almost identical magnetic and structural properties as the single-crystal substrates; this can be explained by the lower surface roughness for thinner underlayer thicknesses. The magnetization saturation ($M_s$) and the ratio $H_{cII}/H_{c{\bot}}$ for the BaM film with a 15 nm MgO (111) underlayer is 217 emu/cc and 0.24, respectively. This is similar to the results for the BaM films deposited on the single-crystal MgO (111) and sapphire substrates of 197 emu/cc and 0.10, 200 emu/cc and 0.12, respectively. Therefore, the proposed MgO (111) underlayer can be used in many applications to promote c-axis orientation without the cost of expensive substrates.

스퍼터링을 이용한 ITO 박막의 저온 증착

  • Jang, Seung-Hyeon;Lee, Yeong-Min;Yang, Ji-Hun;Jeong, Jae-In
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.263-263
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    • 2010
  • 투명도전막(indium tin oxide; ITO)은 투명하면서도 전기 전도도가 높기 때문에, 액정표시소자(LCD; Liquid Crystal Display), 전자발광소자(ELD; Electroluminescent Display) 및 전자 크로믹 소자(Electrochromic Display)를 포함하는 평판형 표시 소자(FPD; Flat Panel Display)와 태양전지 등에 이용되고 있다. 낮은 비저항과 높은 투과율의 ITO 박막은 $300^{\circ}C$ 이상의 고온에서 코팅해야 하는 것으로 알려져 있다. 그러나 최근 플라스틱과 같은 연성 소자가 전자부품에 널리 이용되면서 ITO를 저온에서 증착해야할 필요성이 대두되고 있다. 본 연구에서는 ITO를 플라스틱에 적용하기 위한 저온 코팅 공정 및 시편의 전 후처리공정을 개발하여 박막의 특성을 알아보고자 한다. 실험에 사용된 기판은 고투과율의 고분자(polyethylene terephthalate; PET) 필름이며 $5\;{\times}\;10\;cm^2$의 크기로 절단하여 알코올로 초음파 세척을 실시하였고, 진공 용기에 장입한 후 펄스전원을 이용하여 3분간 in-situ 청정을 실시하였다. ITO 코팅은 마그네트론 스퍼터링을 이용하였으며, 코팅시간, 전처리, 후처리, 기판온도, 산소유량 등 코팅 조건에 따른 박막의 특성을 조사하였다. ITO 박막의 코팅 조건에 따른 박막의 결정구조 분석은 x-선 회절(x-ray diffraction; XRD)을 이용하였고, 박막의 표면형상과 두께 보정 및 단면의 미세조직과 결정 성장 여부 등은 투과전자 현미경(transmission electron microscope; TEM)을 이용하여 분석하였다. 또한 ITO 박막의 면저항과 분광특성은 four-point Probe (CMP-100MP, Advanced Instrument Technology), spectrophotometer (UV-1601, SHIMADZU)를 이용하여 측정하였다. ITO 박막의 광학특성 분석 결과 전광선 투과율은 두께에 따라 변화 하였지만, 색차와 Haze 값은 증착 조건에 따라 큰 차이는 보이지 않았다. 그리고 박막의 결정화에 영향을 주는 가장 중요한 인자는 기판온도이지만, 기판온도를 높이지 못할 경우 비평형 마그네트론(unbalanced-magnetron; UBM)에 의해서 플라즈마 밀도를 높이는 방법으로 유사한 효과를 얻을 수 있음을 확인하였다.

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Optical and Electrical Properties of ZnO Hybrid Structure Grown on Glass Substrate by Metal Organic Chemical Vapor Deposition (유기금속화학증착법으로 유리기판 위에 성장된 산화아연 하이브리드 구조의 광학적 전기적 특성)

  • Kim, Dae-Sik;Kang, Byung Hoon;Lee, Chang-Min;Byun, Dongjin
    • Korean Journal of Materials Research
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    • v.24 no.10
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    • pp.543-549
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    • 2014
  • A zinc oxide (ZnO) hybrid structure was successfully fabricated on a glass substrate by metal organic chemical vapor deposition (MOCVD). In-situ growth of a multi-dimensional ZnO hybrid structure was achieved by adjusting the growth temperature to determine the morphologies of either film or nanorods without any catalysts such as Au, Cu, Co, or Sn. The ZnO hybrid structure was composed of one-dimensional (1D) nanorods grown continuously on the two-dimensional (2D) ZnO film. The ZnO film of 2D mode was grown at a relatively low temperature, whereas the ZnO nanorods of 1D mode were grown at a higher temperature. The change of the morphologies of these materials led to improvements of the electrical and optical properties. The ZnO hybrid structure was characterized using various analytical tools. Scanning electron microscopy (SEM) was used to determine the surface morphology of the nanorods, which had grown well on the thin film. The structural characteristics of the polycrystalline ZnO hybrid grown on amorphous glass substrate were investigated by X-ray diffraction (XRD). Hall-effect measurement and a four-point probe were used to characterize the electrical properties. The hybrid structure was shown to be very effective at improving the electrical and the optical properties, decreasing the sheet resistance and the reflectance, and increasing the transmittance via refractive index (RI) engineering. The ZnO hybrid structure grown by MOCVD is very promising for opto-electronic devices as Photoconductive UV Detectors, anti-reflection coatings (ARC), and transparent conductive oxides (TCO).

Optical properties of epitaxial $Gd_2$O_3:EU^{3+}$luminescent thin films depending on crystallinity ($Gd_2$O_3:EU^{3+}$ 형광체 박막의 결정성에 따른 발광특성 연구)

  • 장문형;최윤기;정권범;황보상우;장홍규;노명근;조만호;손기선;김창해
    • Journal of the Korean Vacuum Society
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    • v.12 no.4
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    • pp.275-280
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    • 2003
  • Epitaxial Gd$_2O_3:Eu^{3+}$luminescent thin films have been grout on Si(III) substrates using ionized Cluster Beam Deposition (ICBD). After the film growing, they were implanted and post annealed to change the crystal structure. The initial growth stage was monitored by using in-situ Reflection High Energy Electron Diffraction (RHEED). The formed crystal structure was identified with X-ray diffraction (XRD) technique and Fourier transform infrared (FT-R) spectroscopy. The electronic states variations were investigated by Near Edge X-ray Absorption Fine Structure (NEXAFS). Photoluminescence (PL), Cathodoluminescence (CL). and Vacuum ultraviolet (VUV) spectrum were used for examining the optical properties. We report the optical property changes depending on crystal structure and the electronic states.

Low Temperature Growth of MCN(M=Ti, Hf) Coating Layers by Plasma Enhanced MOCVD and Study on Their Characteristics (플라즈마 보조 유기금속 화학기상 증착법에 의한 MCN(M=Ti, Hf) 코팅막의 저온성장과 그들의 특성연구)

  • Boo, Jin-Hyo;Heo, Cheol-Ho;Cho, Yong-Ki;Yoon, Joo-Sun;Han, Jeon-G.
    • Journal of the Korean Vacuum Society
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    • v.15 no.6
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    • pp.563-575
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    • 2006
  • Ti(C,N) films are synthesized by pulsed DC plasma enhanced chemical vapor deposition (PEMOCVD) using metal-organic compounds of tetrakis diethylamide titanium at $200-300^{\circ}C$. To compare plasma parameter, in this study, $H_2$ and $He/H_2$ gases are used as carrier gas. The effect of $N_2\;and\;NH_3$ gases as reactive gas is also evaluated in reduction of C content of the films. Radical formation and ionization behaviors in plasma are analyzed in-situ by optical emission spectroscopy (OES) at various pulsed bias voltages and gas species. He and $H_2$ mixture is very effective in enhancing ionization of radicals, especially for the $N_2$. Ammonia $(NH_3)$ gas also highly reduces the formation of CN radical, thereby decreasing C content of Ti(C, N) films in a great deal. The microhardness of film is obtained to be $1,250\;Hk_{0.01}\;to\;1,760\;Hk_{0.01}$ depending on gas species and bias voltage. Higher hardness can be obtained under the conditions of $H_2\;and\;N_2$ gases as well as bias voltage of 600 V. Hf(C, N) films were also obtained by pulsed DC PEMOCYB from tetrakis diethyl-amide hafnium and $N_2/He-H_2$ mixture. The depositions were carried out at temperature of below $300^{\circ}C$, total chamber pressure of 1 Torr and varying the deposition parameters. Influences of the nitrogen contents in the plasma decreased the growth rate and attributed to amorphous components, to the high carbon content of the film. In XRD analysis the domain lattice plain was (111) direction and the maximum microhardness was observed to be $2,460\;Hk_{0.025}$ for a Hf(C,N) film grown under -600 V and 0.1 flow rate of nitrogen. The optical emission spectra measured during PEMOCVD processes of Hf(C, N) film growth were also discussed. $N_2,\;N_2^+$, H, He, CH, CN radicals and metal species(Hf) were detected and CH, CN radicals that make an important role of total PEMOCVD process increased carbon content.