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Sintering Behavior of $TiB_2$-SiC Composites ($TiB_2$-SiC 복합재료의 소결거동)

  • 윤재돈
    • Journal of Powder Materials
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    • v.1 no.1
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    • pp.15-20
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    • 1994
  • The effect of SiC addition on sintering behaviors and microstructures of TiB2 ceramics were studied. The sintering of TiB2 was limited due to the surface diffusion and rapid grain growth at high temperature. However the addition of SiC to TiB2 ceramics improved the densification to above 99% of the theoretical density. The sintering of TiB2-SiC composite starts at 120$0^{\circ}C$ with the melting of the oxides in particle surface as impurities. After the reduction of the oxide by additional cabon at above 140$0^{\circ}C$, the grain boundary diffusion through the interface of TiB2-SiC play an important role. TEM observation showed neither chemical reactions nor other phases formed at the TiB2-SiC interfaces but the microcracks were observed due to the mismatch of thermal expansion between TiB2-SiC.

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Chemical Binding States of Ti and O Elements in Anodic Ti Oxide Films (Ti 양극산화 피막에서 Ti 및 O원소의 화학결합 상태)

  • 유창우;오한준;이종호;장재명;지충수
    • Journal of the Korean institute of surface engineering
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    • v.35 no.6
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    • pp.383-390
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    • 2002
  • To investigate behaviors of Ti and O elements and microstructures of anodic titanium oxide films, the films were prepared by anodizing pure titanium in $H_2$S $O_4$, $H_3$P $O_4$, and $H_2O$$_2$ mixed solution at 180V. The microstructures and chemical states of the elements were analyzed using SEM, X-ray mapping, AFM, XRD, XPS (depth profile). The films formed on a titanium substrate showed porous layers which were composed of pore and wall, And with increasing anodizing time a hexagonal shape of cell structures were dominant and solace roughness increased. From the XRD result the structure of the Ti $O_2$ layer was anatase type of crystal on the whole. In the XPS spectra it was found that Ti and O were chemically binded in forms of Ti $O_2$, TiOH, $Ti_2$ $O_3$ at Ti 2p, and Ti $O_2$, $Ti_2$ $O_3$, $P_2$ $O_{5}$, S $O_4^{2-}$ at O ls respectively. Concentration of Ti $O_2$ decreased as the depth increased from the surface of the oxide film towards the substrate, but to the contrary concentrations of TiOH and $Ti_2$ $O_3$ increased.d.

Property of the Nano-Thick TiO2 Films Using an ALD at Low Temperature (저온 ALD로 제조된 TiO2 나노 박막 물성 연구)

  • Yoon, Ki-Jeong;Song, Oh-Sung
    • Korean Journal of Materials Research
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    • v.18 no.10
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    • pp.515-520
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    • 2008
  • We fabricated 10 nm-$TiO_2$ thin films for DSSC (dye sensitized solar cell) electrode application using ALD (atomic layer deposition) method at the low temperatures of $150^{\circ}\;and\;250^{\circ}$. We characterized the crosssectional microstructure, phase, chemical binding energy, and absorption of the $TiO_2$ using TEM, HRXRD, XPS, and UV-VIS-NIR, respectively. TEM analysis showed a 10 nm-thick flat and uniform $TiO_2$ thin film regardless of the deposition temperatures. Through XPS analysis, it was found that the stoichiometric $TiO_2$ phase was formed and confirmed by measuring main characteristic peaks of Ti $2p^1$, Ti $2p^3$, and O 1s indicating the binding energy status. Through UV-VIS-NIR analysis, ALD-$TiO_2$ thin films were found to have a band gap of 3.4 eV resulting in the absorption edges at 360 nm, while the conventional $TiO_2$ films had a band gap of 3.0 eV (rutile)${\sim}$3.2 eV (anatase) with the absorption edges at 380 nm and 410 nm. Our results implied that the newly proposed nano-thick $TiO_2$ film using an ALD process at $150^{\circ}$ had almost the same properties as thsose of film at $250^{\circ}$. Therefore, we confirmed that the ALD-processed $TiO_2$ thin film with nano-thickness formed at low temperatures might be suitable for the electrode process of flexible devices.

Hydrothermal Synthesis and Characterization of BaTiO3 Fine Powders (BaTiO3 미세 분말의 수열합성 및 특성분석)

  • Park, Jung-Hoon;Park, Sangdo
    • Korean Chemical Engineering Research
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    • v.45 no.5
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    • pp.448-454
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    • 2007
  • Hydrothermal synthesis was conducted with starting material as Barium hydroxide and hydrous titania ($TiO_2{\cdot}xH_2O$) to obtain barium titanate fine Powder. The conversion, crystal structure and properties of as-prepared powder were investigated according to reaction temperature, time and concentration. The effect of variables on conversion was in order of time < temperature < concentration and the maximum conversion reached to 99.5% in the case of hydrothermal synthesis at $180^{\circ}C$ for 2 h with 2.0 M reactant concentration. At low concentration such as 0.25 M, formation of unreacted $BaCO_3$ and $TiO_2$ was not inevitable at even high reaction temperature and these components converted into $BaTi_2O_5$ at high temperature and remained as impurity. As concentration of reactant increased, the size of as-synthesized $BaTiO_3$ powder deceased and Ba/Ti molar ratio approached into 1, showing Ba/Ti ratio of $1{\pm}0.005$ for reaction at $180^{\circ}C$ for 2 h with 2.0 M concentration.

Forming Characteristics for the Bundle Extrusion of Cu-Ti Bimetal Wires (구리-타이타늄 복합선재의 번들압출 성형특성)

  • Lee, Y.S.;Kim, J.S.;Yoon, S.H.;Lee, H.Y.
    • Transactions of Materials Processing
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    • v.18 no.4
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    • pp.342-346
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    • 2009
  • Forming characteristics for the bundle extrusion of Cu-Ti bimetal wires are investigated, which can identify the process conditions for weak mechanical bonding at the contact surface during the direct extrusion of a Cu-Ti bimetal wire bundle. Bonding mechanism between Cu and Ti is assumed as a cold pressure welding. Then, the plastic deformation at the contact zone causes mechanical bonding and a new bonding criterion for pressure welding is developed as a function of the principal stretch ratio and normal pressure at the contact surface by analyzing micro local extrusion at the contact zone. The averaged deformation behavior of Cu-Ti bimetal wire is adopted as a constitutive behavior at a material point in the finite element analysis of Cu-Ti wire bundle extrusion. Various process conditions for bundle extrusions are examined. The deformation histories at the three points, near the surface, in the middle and near the center, in the cross section of a bundle are traced and the proposed new bonding criterion is applied to predict whether the mechanical bonding at the Cu-Ti contact surface happens. Finally, a process map for the direct extrusion of Cu-Ti bimetal wire bundle is proposed.

Microstructure and Dielectric Properties of $BaTi_4O_9$ Thin Film for Microwave Devices (고주파 소자용 $BaTi_4O_9$ 박막의 미세구조와 유전특성 연구)

  • Jang, Bo-Yun;Lee, Suk-Jin;Nahm, Sahn;Lee, Hwack-Joo
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.07a
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    • pp.125-129
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    • 2004
  • [ $BaTi_4O_9$ ] thin film were grown on $Pt/Ti/SiO_2/Si$ substrate using rf magnetron sputter, and the microstructure and dielectric properties of the thin films were investigated. For the film grown at $350^{\circ}C$ and rapidly thermal annealed at $900^{\circ}C$, the $BaTi_5O_{11}$ Phase was formed. However, the $BaTi_4O_9$ phase was formed when the growing temperature exceeded $450^{\circ}C$ The dielectric constant of the $BaTi_4O_9$ thin film grown at $550^{\circ}C$ and rapidly thermal annealed at $900^{\circ}C$ was about 40 at low frequency range($100kHz{\sim}1MHz$) and 36 at microwave range($1{\sim}10GHz$) which is very close to that of the bulk $BaTi_4O_9$ phase. The dissipation factor was very low, about 0.005 at low frequency as well as microwave range.

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Synthesis Behavior of Ti-25.0~37.5at%Si Powders by In situ Thermal Analysis during Mechanical Alloying (기계적 합금화과정에서의 in situ 열분석에 의한 Ti-25.0~37.5at%Si 분말의 합성거동)

  • Byun Chang Sop;Hyun Chang Yong;Kim Dong Kwan
    • Korean Journal of Materials Research
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    • v.14 no.5
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    • pp.305-309
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    • 2004
  • Mechanical alloying (MA) of Ti-25.0~37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0~26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1~37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1~37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

Effect of Ti Concentration on the Microstructure of Al and the Tunnel Magnetoresistance Behaviors of the Magnetic Tunnel Junction with a Ti-alloyed Al-oxide Barrier (Ti 첨가에 따른 Al 미세구조 변화 효과와 산화 TiAl 절연층을 갖는 자기터널접합의 자기저항 특성)

  • Song, Jin-Oh;Lee, Seong-Rae
    • Journal of the Korean Magnetics Society
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    • v.15 no.6
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    • pp.311-314
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    • 2005
  • We investigated the composition dependence of the tunneling magnetoresistance (TMR) behavior and the stability of the magnetic tunnel junctions (MTJs) with TiAlOx barrier and the microstructural evolution of TiAl alloy films. The TMR ratio increased up to $49\%$ at $5.33\;at\%$ Ti. In addition, a significant tunneling magnetoresistance (TMR) value of $20\%$ was maintained after annealing at $450^{\circ}C$, and the breakdown voltage ($V_B$) of and 1.35 V were obtained in the MTJ with $5.33\;at\%$ Ti-alloyed AlOx barrier. These results were closely related to the enhanced quality of the barrier material microstructure in the pre-oxidation state. Ti alloying enhanced the barrier/electrode interface uniformity and reduced microstructural defects. These structural improvements enhanced not only the TMR effect but also the thermal and electrical stability of the MTJs.

Photodecomposition of Concentrated Ammonia over Nanometer-sized TiO2, V-TiO2, and Pt/V-TiO2 Photocatalysts

  • Choi, Hyung-Joo;Kim, Jun-Sik;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.581-588
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    • 2007
  • To enhance the photodecomposition of concentrated ammonia into N2, Pt/V-TiO2 photocatalysts were prepared using solvothermal and impregnation methods. Nanometer-sized particles of 0.1, 0.5 and 1.0 mol% V-TiO2 were prepared solvothermally, and then impregnated with 1.0 wt% Pt. The X-ray diffraction (XRD) peaks assigned to V2O5 at 30.20 (010) and Pt metal at 39.80 (111) and 46.20 (200) were seen in the 1.0 wt% Pt/ 10.0 mol% V-TiO2. The particle size increased in the order: pure TiO2, V-TiO2 and Pt/V-TiO2 after thermal treatment at 500 °C, while their surface areas were in the reverse order. On X-ray photoelectron spectroscopy (XPS), the bands assigned to the Ti2p3/2 and Ti2p1/2 of Ti4+-O were seen in all the photocatalysts, and the binding energies increased in the order: TiO2 < Pt/V-TiO2 < V-TiO2. The XPS bands assigned to the V2p3/2 (517.85, 519.35, and 520.55 eV) and V2p1/2 (524.90 eV) in the V3+, V4+ and V5+ oxides appeared over V-TiO2, respectively, while the band shifted to a lower binding energy with Pt impregnation. The Pt components of Pt/ V-TiO2 were identified at 71.60, 73.80, 75.00 and 76.90 eV, which were assigned to metallic Pt 4f7/2, PtO 4f7/2, PtO2 4f7/2, and PtO 4f5/2, respectively. The UV-visible absorption band shifted closer towards the visible region of the spectrum in V-TiO2 than in pure TiO2 and; surprisingly, the Pt/V-TiO2 absorbed at all wavelengths from 200 to 800 nm. The addition of vanadium generated a new acid site in the framework of TiO2, and the medium acidic site increased with Pt impregnation. The NH3 decomposition increased with the amount of vanadium compared to pure TiO2, and was enhanced with Pt impregnation. NH3 decomposition of 100% was attained over 1.0 wt% Pt/1.0 mol% V-TiO2 after 80 min under illumination with 365 nm light, although about 10% of the ammonia was converted into undesirable NO2 and NO. Various intermediates, such as NO2, -NH2, -NH and NO, were also identified in the Fourier transform infrared (FT-IR) spectra. From the gas chromatography (GC), FT-IR and GC/mass spectroscopy (GC/MS) analyses, partially oxidized NO and NO2 were found to predominate over V-TiO2 and pure TiO2, respectively, while both molecules were reduced over Pt/V-TiO2.

Acidic Properties and Catalytic Activity of Titanium Sulfate Supported on TiO2

  • Sohn, Jong-Rack;Lee, Si-Hoon;Cheon, Park-Won;Kim, Hea-Won
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.657-664
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    • 2004
  • Titanium sulfate supported on $TiO_2$was prepared by impregnation of powdered $TiO_2$with an aqueous solution of titanium sulfate followed by calcining in air at high temperature. For Ti$(SO_4)_2/TiO_2$ samples calcined at 300 $^{\circ}C$, no diffraction lines of titanium sulfate are observed at $Ti(SO_4)_2$loading up to 30 wt%, indicating good dispersion of $Ti(SO_4)_2$ on the surface of $TiO_2$. The acidity of the catalysts increased in proportion to the titanium sulfate content up to 20 wt% of $Ti(SO_4)_2$. 20 wt% $Ti(SO_4)_2/TiO_2$ calcined at 300 $^{\circ}C$ exhibited maximum catalytic activities for 2-propanol dehydration and cumene dealkylation. The catalytic activities for these reactions, were correlated with the acidity of catalysts measured by ammonia chemisorption method.