• Title/Summary/Keyword: Rutile phase

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SURFACE CHARACTERISTICS AND BIOACTIVITY OF ANODICALLY OXIDIZED TITANIUM SURFACES (양극산화에 의한 티타늄 산화막의 표면 특성 및 생체 활성에 관한 연구)

  • Lee, Sang-Han;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.45 no.1
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    • pp.85-97
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    • 2007
  • Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

Effect of Alloy Addition (Ta, Nb) on Oxidation Behavior of cp-Ti for Biomaterials (생체용 Ti합금의 산화거동에 미치는 Ta 및 Nb 첨가의 영향)

  • Lee Doh-Jae;Oh Tae-Wook;Park Bum-Su;Kim Soo-Hak;Jun Choong-Geug;Yoon Kye-Lim
    • Korean Journal of Materials Research
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    • v.14 no.3
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    • pp.211-217
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    • 2004
  • The oxidation behaviors of Ti-10Ta-10Nb alloy and Ti-6Al-4V alloy were studied in dry air atmosphere. Specimens were melted in consumable vacuum arc furnace and homogenized at $1050^{\circ}C$ for 24 h. Hot rolling was performed at $1000^{\circ}C$. Specimens of the alloys were oxidized as the temperature range $400~650^{\circ}C$ for 30 min. The oxidation behavior of the alloys was analysed by optical microscope, SEM/EDX, XRD, XPS and TGA. Immersion test was performed in 1% Lactic acid. In the microscope observation, oxide layer of Ti-10Ta-10Nb alloy was denser and thinner than Ti-6Al-4V's. The weight gains during the oxidation rapidly increased at the temperature above $600^{\circ}C$ in Ti-6Al-4V's alloy and$ 700^{\circ}C$ in Ti-10Ta-10Nb alloy. According to XRD results, oxide layers were composed of mostly $TiO_2$(rutile) phase. It was analysed that the passive film of the Ti alloys consisted of $TiO_2$ through X-ray photoelectron spectroscopy(XPS) analysis.

Photoelectrocatalytic Degradation of Dyes in Aqueous Solution Using CNT/TiO2 Electrode

  • Zhang, Feng-Jun;Liu, Jin;Chen, Ming-Liang;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.46 no.3
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    • pp.263-270
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    • 2009
  • The effect of photoelectrocatalytic (PEC) degradation for different dyes with the CNT/$TiO_2$ electrode was studied. The prepared electrode was characterized with surface properties, structural crystallinity, elemental identification, and PEC activity. The $N_2$ adsorption data showed that the composites had decreased surface area compared with the pristine CNT. This indicated the blocking of micropores on the surface of CNT, which was further supported by observation via FESEM. XRD patterns of the composites showed that the CNT/$TiO_2$ composite contained a mixing anatase and rutile phase. EDX spectra showed the presence of C, O and Ti peaks for all samples. The decomposition efifciency of the prepared electrode was evaluated by the PEC degradation of three dyes (methylene blue (MB), rhodamine B (RH.B), methyl orange (MO)). The variations of the FT-IR spectra and pH value of dye solutions were measured during the PEC system; it was found that the CNT/$TiO_2$ electrode has better PEC degradation for MB solution than that of RH.B and MO. The proposed degradation mechanism was present.

Improvement of Light-Harvesting Efficiency of TiO2 Granules Through Chemical Interconnection of Nanoparticles by Adding TEOT to Spray Solution

  • Lim, Mi Ja;Song, Shin Ae;Kang, Yun Chan;So, Won-Wook;Jung, Kyeong Youl
    • Korean Chemical Engineering Research
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    • v.53 no.5
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    • pp.632-637
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    • 2015
  • Mesoporous $TiO_2$ granules were prepared by spray pyrolysis using nano-sized titania particles which were synthesized by a hydrothermal method, and they were evaluated as the photoanode of dye-sensitized solar cells. To enhance the cell efficiency, nanoparticles within granules were chemically interconnected by adding titanium ethoxide (TEOT) to colloidal spray solution. The resulting titania particles had anatase phase without forming rutile. $TiO_2$ granules obtained showed about 400 nm in size, the specific surface area of $74-77m^2/g$, and average pore size of 13-17 nm. The chemical modification of $TiO_2$ granules by adding TEOT initially to the colloidal spray solution was proved to be an effective way in terms of increasing both the light scattering within photoanode and the lifetimes of photo-excited electrons. Consequently, the light-harvesting efficiency of TEOT-modified granules (${\eta}=6.72%$) was enhanced about 14% higher than primitive nanoparticles.

Characterization and Photonic Effect of Novel Ag-CNT/TiO2 Composites and their Bactericidal Activities

  • Zhang, Feng-Jun;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1981-1987
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    • 2010
  • A novel composite (Ag-CNT/$TiO_2$) of silver treated carbon nanotubes (Ag-CNT) and $TiO_2$ was synthesized via wet chemistry followed by a heat treatment. The dispersion and structure of the silver in the synthesized composites determined by X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy(TEM). XRD patterns of the composites showed that the composites contained a mixing anatase and rutile phase. The EDX spectra showed the presence of C, O, Ti and Ag peaks. The $TiO_2$ particles were distributed uniformly in the CNT network, and silver particles were virtually fixed on the surface of the tube. The photocatalysis degraded behaviors of the Ag-CNT/$TiO_2$ composites of the methylene blue, which increased with an increase of the silver component. The Ag-CNT/$TiO_2$ composites have excellent antibacterial activities against Escherichia coli (E. Coli), Pseudomonas aeruginosa (P. Aeru) and Bacillus subtilis (B. Sub) under visible light.

A study on the nature of needle-like inclusions in corundum crystals (커런덤의 침상내포물 본질에 관한 연구)

  • 배상덕;김상기;최종건;김판채
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.3
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    • pp.101-104
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    • 2004
  • It was realized that MC-XRD is useful for phase analyzing of inclusions in crystals because it can focus the X-Ray beam to the small particles sized dozens of $\mu\textrm{m}$ with high S/N ratio. By using this MC-XRD, needle-like inclusions which are seen generally in corundum crystals known as rutile was found to be the iron titanium oxide and iron oxide which has the chemical composition of $Fe_2TiO_4,\; Fe_2TiO_5,\; Fe_2O_3$respectively

Synthesis of ultrafine particles and thin films of $SnO_2$ by the spray-ICP technique (Spray-ICP technique에 의한 $SnO_2$미분말 합성 및 박막 제조)

  • 김정환;박종현;김영도;신건철
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.3
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    • pp.487-492
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    • 1998
  • Ultrafine particles of $SnO_2$ or $(Sn,Ti)O_2$ and thin films of $SnO_2$ were synthesized by introducing aqueous tin chloride solution into a high temperature argon inductively coupled plasma (ICP) generated under ambient pressure (the spray-ICP technique). As-deposited $SnO_2$ particles from each concentration of solution were all tetragonal $SnO_2$ crystallline phase and their mean size decreased in proportion to the increase of solution concentration. The mean size of $SnO_2$ particles was in the 10~40 nm range.

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In-situ monitoring of oxidation states of vanadium with ambient pressure XPS

  • Kim, Geonhwa;Yoon, Joonseok;Yang, Hyukjun;Lim, Hojoon;Lee, Hyungcheol;Jeong, Changkil;Yun, Hyungjoong;Jeong, Beomgyun;Ethan, Crumlin;Lee, Juhan;Ju, Honglyoul;Mun, Bongjin Simon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.125.2-125.2
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    • 2015
  • The evolution of oxidation states of vanadium is monitored with ambient pressure X-ray photoemission spectroscopy. As the pressure of oxygen gas and surface temperature change, the formations of various oxidation states of vanadium are observed on the surface. Under 100mTorr of the oxygen gas pressure and 523K of sample temperature, VO2 and V2O5 are formed on the surface. The temperature-dependent resistance measurement on grown sample shows a clear metal-insulator transition near 350K. In addition, the measurement of Raman spectroscopy displays the structural change from monoclinic to rutile structures across the phase transition temperature.

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Annealing Effect on the Crystal Structure of $TiO_2$ Thin Film (이산화티타늄 박막의 열처리에 따른 결정구조 분석)

  • Kim, Seon-Hoon;Yang, Myung-Hak;Kim, Tae-Un;Ki, Hyun-Chul;Kim, Doo-Gun;Han, Myung-Soo;Ko, Hang-Ju;Kim, Hyo-Jin;Kim, Hwe-Jong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.213-213
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    • 2009
  • Titanium dioxide ($TiO_2$) thin films were prepared on glass substrates by ion-assisted electron-beam evaporation with 200nm thickness and subsequently crystallized by rapid thermal annealing at the rage of $200{\sim}700^{\circ}C$ in flowing $N_2$ gas. The crystal structure of the films were examined by X-ray diffractometer. As-deposited $TiO_2$ films were amorphous. After annealing, anatase and rutile phase of $TiO_2$ films were observed together.

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Titanium Oxide Film : A New Biomaterial For Artificial Heart Valve Prepared by Ion Beam Enhanced Deposition

  • Liu, Xianghuai;Zhang, Feng;Zheng, Zhihong;Huang, Nan
    • Journal of the Korean Vacuum Society
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    • v.6 no.S1
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    • pp.1-15
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    • 1997
  • Titanium oxide films were prepared by ion beam enhanced deposition where the films were synthesized by deposition titianium atoms and simultaneously bombarding with xenon ion beam at an energy of 40 keV in an $O_2$ environ,ent. Structure and composition of titanium oxide films were investigated by X-ray Doffractopm (XRD) Ritjerfprd Backscattering Spectroscopy (RBS) and X-ray Diffraction(XRD) Rutherford Backscattering Spectroscopy (RBS) and X-ray photoelectron spectroscopy (XPS) The results show that thestructure of the prepared films exhibit a rutile phase structure wit high(200) orientation and the O/Ti ratio of the titanium oxide films was about 2:1 XPS anlysis shows that $Ti^{2+},Ti^{3+}\;and\;Ti^{4+}$ chemical states exist on the titanium oxide films. the blood compatibility of the titanium oxide films was studied by measurements of blood clotting time and platelet adhesion. The results show that the anticoagulation property of titanium oxide films improved significantly and better than that of LTI-carbon which was widely used to fabricate artificial heart valve.

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