• 한국재료학회지
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• 제9권5호
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• pp.503-508
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• 1999

We have investigated the physical and diffusion barrier property of Ti-Si-N film for Cu metallization. The ternary compound was deposited by using reactive rf magnetron sputtering of a TiSi$_2$target in an Ar/$N_2$gas mixture. Resistivities of the films were in range of 358$\mu$$\Omega$-cm, to 307941$\mu$$\Omega$-cm, and tended to increase with increasing the $N_2$/Ar flow rate ratio. The crystallization of the Ti-Si-N compound started to occur at 100$0^{\circ}C$ with the phases of TiN and Si$_3$N$_4$identified by using XRD(X-ray Diffractometer). The degree of the crystallization was influenced by the $N_2$/Ar flow ratio. The diffusion barrier property of Ti-Si-N film for Cu metallization was determined by AES, XRD and etch pit by secco etching, revealing the failure temperature of 90$0^{\circ}C$ in 43~45at% of nitrogen content. In addition, the very thin compound (10nm) with 43~45at% nitrogen content remained stable up to $700^{\circ}C$. Furthermore, thermal treatment in vacuum at $600^{\circ}C$ improved the barrier property of the Ti-Si-N film deposited at the $N_2$(Ar+$N_2$) ratio of 0.05. The addition of Ti interlayer between Ti-Si-N films caused the drastic decrease of the resistivity with slight degradation of diffusion barrier properties of the compound.

• 한국세라믹학회지
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• 제30권2호
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• pp.148-156
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• 1993

TiN films were deposited onto high speed steel (SKH9) by plasma assisted chemical vapor deposition (PACVD) using a TiCl4/N2/H2/Ar gas mixture at around 50$0^{\circ}C$. The effects of the deposition temperature, R.F. power and TiCl4 concentration on the deposition of TiN and the microhardness of TiN film were investigated. The crystallinity and the microhardness of TiN films were improved with increase of the deposition temperature. Optimum deposition temperature in this study was 50$0^{\circ}C$, because a softening or phase transformation of the substrate occurred over 50$0^{\circ}C$. A large increase of the film growth rate with a strong(200) preferred orientation was obtained by increasing R.F. power. Much chlorine content of about 10at.% was found in the deposited films and resulted in relatively low average microhardness of about 1, 500Kgf/$\textrm{mm}^2$ compared with the theoretical value(~2, 000Kgf/$\textrm{mm}^2$).

• 전자공학회논문지A
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• 제29A권7호
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• pp.73-81
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• 1992

We have investigated the thermal reaction property and the oxygen behavior of TiN/Ti/Si structure after different hear treatments using x-ray photoelectron spectroscopy and cross-sectional transmission electron microscopy measurements. During the heat treatment in N$_2$ amibient, the considerable amount of oxygen atoms incorporates into TiN/Ti/Si Structures. It is found that oxygen atoms pile up at the top surface of TiN and TiN/Ti interface, forming a compound of TiO$_2$ above $600^{\circ}C$. Inside the TiN film, the oxygen content increases as the annealing temperature increases, mostly TiO and Ti$_2$O$_3$ rather than thermodynamically stable TiO$_2$. Above the annealing temperature of 55$0^{\circ}C$, the TiSi$_2$ formation has initiated. One thing to note is that a severe blistering is observed in the sample annealed at $600^{\circ}C$, due to (1) the difference of thermal expansion coefficient between TiN and Si` (2) the compressive stress induced by the volume reduction caused by the Ti-Silicide grain while elevating temperatures.

• 소성∙가공
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• 제15권8호
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• pp.581-585
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• 2006

Effects of V on both the formation of Ti-Nb-V carbonitrides and mechanical properties of Ti-Nb bearing low carbon HSLA steels were investigated. Hot rolling process was simulated by using Gleeble 3500 system with the steels containing three different levels of V ($0{\sim}0.1wt.%$). Vanadium precipitated as Ti-Nb-V carbonitrides at austenite region but it did not precipitate as VC during austenite to acicular ferrite or bainitic ferrite phase transformation. As V content increased, the amount of Nb precipitates was decreased but the average size of Ti-Nb-V carbonitrides was increased due to larger diffusivity of V than that of Nb. Coarsened Ti-Nb-V carbonitrides could act as heterogeneous nucleation site during ${\gamma}{\rightarrow}{\alpha}$ phase transformation, thus, acicular ferrite transformation was promoted as V content increased, resulting in increase of upper shelf energy.

• 한국표면공학회지
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• 제41권2호
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• pp.69-75
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• 2008

Electrochemical behaviors of surface modified and MC3T3-E1 cell cultured Ti-30Ta alloys have been investigated using various electrochemical methods. The Ti alloys containing Ta were melted by using a vacuum furnace and then homogenized for 6 hrs at $1000^{\circ}C$. MC3T3-E1 cell culture was performed with MC3T3-E1 mouse osteoblasts for 2 days. The microstructures and corrosion resistance were measured using FE-SEM, XRD, EIS and potentiodynamic test in artificial saliva solution at $36.5{\pm}1^{\circ}C$. Ti-Ta alloy showed the martensite structure of ${\alpha}+{\beta}$ phase and micro-structure was changed from lamellar structure to needle-like structure as Ta content increased. Corrosion resistance increased as Ta content increased. Corrosion resistance of cell cultured Ti-Ta alloy increased predominantly in compared with non cell cultured Ti- Ta alloy due to inhibition of the dissolution of metal ion by covered cell. $R_p$ value of MC3T3-E1 cell cultured Ti-40 Ta alloy showed $1.60{\times}10^6{\Omega}cm^2$ which was higher than those of other Ti alloy. Polarization resistance of cell-cultured Ti-Ta alloy increased in compared with non-cell cultured Ti alloy.

• 한국진공학회:학술대회논문집
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• 한국진공학회 1999년도 제17회 학술발표회 논문개요집
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• pp.211-211
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• 1999

Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

• Corrosion Science and Technology
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• 제8권4호
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• pp.143-147
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• 2009

In biomedical implants and dental fields, titanium has been widely utilized for excellent corrosion resistance and biocompatibility. However, Ti and its alloys are nonbioactive after being implanted in bone. In this study, for the purpose of improvement in biocompatibility the anodic $TiO_2$ layer on Ti-xNb alloys were fabricated by electrochemical method in phosphate solution, and the effect of Nb content on the pore size, the morphology and crystallinity of Ti oxide layer formed by the anodic oxidation method was investigated. The Ti containing Nb up to 3 wt%, 20 wt% and 40 wt% were melted by using a vacuum furnace. The sample were cut, polished, and homogenized for 24 hr at $1050^{\circ}C$ for surface roughness test and anodizing. Titanium anodic layer was formed on the specimen surface in an electrolytic solution of 1 M phosphoric acid at constant current densities ($30mA/cm^2$) by anodizing method. Microstructural morphology, crystallinity, composition, and surface roughness of oxide layer were observed by FE-SEM, XRD, EDS, and roughness tester, respectively. The structure of alloy was changed from $\alpha$-phase to $\beta$-phase with increase of Nb content. From XRD results, the structure of $TiO_2$ formed on the Ti-xNb surface was anatase, and no peaks of $Nb_2O_5$ or other Nb oxide were detected suggesting that Nb atoms are dispersed in $TiO_2$-based solid solution. Surface roughness test and SEM results, pore size formed on surface and surface roughness decreased as Nb content increased. From the line analysis results, intensity of Ti peak was high in the center of pore, whereas, intensity of O peak was high in the outside of pore center.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2012년도 춘계학술발표회 논문집
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• pp.254-254
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• 2012

The purposed of this work was to determine surface charateristics of anodized Ti-30Nb-xTa alloys with Ta content. Samples were prepared by arc melting, followed by followed by homogenization for 12 hr at $1000^{\circ}C$ in argon atmosphere. The electrolyte for anodization treatment was prepared by mixing 465ml $H_2O$ with 35M $H_3PO_4$ and anodized at 180V to 220V. The microstructures of the alloys were examined by X-ray diffractometer (XRD) and optical microscopy (OM). Surface characteristics of anodized Ti-30Nb-xTa alloys was investigated by potentiodynamic test and potentiostatic in 0.9% Nacl solution at $36.5{\pm}1^{\circ}C$. It was observed that the changed ${\alpha}$ phase to ${\beta}$ phase with Ta content.

• 한국재료학회지
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• 제22권7호
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• pp.352-357
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• 2012

$SnO_2$-mixed and Sn-doped $TiO_2$ nanoparticles were synthesized via a hydrothermal process. $SnO_2$-mixed $TiO_2$ nanoparticles prepared in a neutral condition consisted of anatase $TiO_2$ nanoparticles(diamond shape, ~25 nm) and cassiterite $SnO_2$ nanoparticles(spherical shape, ~10 nm). On the other hand, Sn-doped $TiO_2$ nanoparticles obtained under a high acidic condition showed a crystalline phase corresponding to rutile $TiO_2$. As the Sn content increased, the particle shape changed from rod-like(d~40 nm, 1~200 nm) to spherical(18 nm) with a decrease in the particle size. The peak shift in the XRD results and a change of the c-axis lattice parameter with the Sn content demonstrate that the $TiO_2$ in the rutile phase was doped with Sn. The photocatalytic activity of the $SnO_2$-mixed $TiO_2$ nanoparticles dramatically increased and then decreased when the $SnO_2$ content exceeded 4%. The increased photocatalytic activity is mainly attributed to the improved charge separation of the $TiO_2$ nanoparticles with the $SnO_2$. In the case of Sn-doped $TiO_2$ nanoparticles, the photocatalytic activity increased slightly with the Sn content due most likely to the larger energy bandgap caused by Sn-doping and the decrease in the particle size. The $SnO_2$-mixed $TiO_2$ nanoparticles generally exhibited higher photocatalytic activity than the Sn-doped $TiO_2$ nanoparticles. This was caused by the phase difference of $TiO_2$.

• 한국수소및신에너지학회논문집
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• 제10권4호
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• pp.197-210
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• 1999

The hydrogen storage performance and electrochemical properties of $Zr_{1-X}Ti_X(Mn_{0.2}V_{0.2}Ni_{0.6})_{1.8}$(X=0.0, 0.2, 0.4, 0.6) alloys are investigated. The relationship between discharge performance and alloy characteristics such as P-C-T characteristics and crystallographic parameters is also discussed. All of these alloys are found to have mainly a C14-type Laves phase structure by X-ray diffraction analysis. As the mole fraction of Ti in the alloy increases, the reversible hydrogen storage capacity decreases while the equilibrium hydrogen pressure of alloy increases. Furthermore, the discharge capacity shows a maxima behavior and the rate-capability is increased, but the cycling durability is rapidly degraded with increasing Ti content in the alloy. In order to analyze the above phenomena, the phase distribution, surface composition, and dissolution amount of alloy constituting elements are examined by S.E.M., A.E.S. and I.C.P. respectively. The decrease of secondary phase amount with increasing Ti content in the alloy explains that the micro-galvanic corrosion by multiphase formation is little related with the degradation of the alloys. The analysis of surface composition shows that the rapid degradation of Ti-substituted Zr base alloy electrode is due to the growth of oxygen penetration layer. After comparing the radii of atoms and ions in the electrolyte, it is clear that the electrode surface becomes more porous, and that is the source of growth of oxygen penetration layer while accelerating the dissolution of alloy constituting elements with increasing Ti content. Consequently, the rapid degradation (fast growth of the oxygen-penetrated layer) with increasing Ti substitution in Zr-based alloy is ascribed to the formation of porous surface oxide through which the oxygen atom and hydroxyl ion with relatively large radius can easily transport into the electrode surface.