• Korean Journal of Materials Research
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• v.9 no.5
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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.

• International Journal of Ocean System Engineering
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• v.2 no.2
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• pp.106-115
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• 2012

In the present study, TiN and CrN films were coated by arc ion plating equipment onto aluminum alloy substrate, A2024. The film thickness was about 4.65 ${\mu}m$. TiN and CrN films were analyzed by X-ray diffraction and energy dispersive X-ray equipments. The Young's modulus and the micro-Vickers hardness of aluminum substrate were modified by the ceramic film coatings. The difference in Young's modulus between substrate and coating film would affect on the wear resistance. The critical load, Lc, was 75.8 N for TiN and 85.5 N for CrN. It indicated from the observation of optical micrographs for TiN and CrN films that lots of cracks widely propagated toward the both sides of scratch track in the early stage of MODE I. TiN film began to delaminate completely at MODE II stage. The substrate was finally glittered at MODE III stage. For CrN film, a few crack can be observed at MODE I stage. The delamination of film was not still occurred at MODE II and then was happened at MODE III. This agrees with critical load measurement which the adhesive strength was greater for CrN film than for TiN film. Consequently, it was difficult for CrN to delaminate because the adhesive strength was excellent against Al substrate. The wear process, which the film adheres and the ball transfers, could be enhanced because of the increase in loading. The wear weight of ball was less for CrN than for TiN. This means that the wear damage of ball was greater for TiN than for CrN film. It is also obvious that it was difficult to delaminate because the CrN coating film has high toughness. The coefficient of friction was less for CrN coating film than for TiN film.

• Journal of the Korean Society for Heat Treatment
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• v.36 no.2
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• pp.61-68
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• 2023

Ti and Ti alloys are used in the automobile and aerospace industries due to their high specific strength and excellent corrosion resistance. However their application is limited due to poor formability at room temperature and high unit cost. In order to overcome these issues, dissimilarly jointed materials, such as cladding materials, are widely investigated to utilize them in each industrial field because of an enhanced plasticity and relatively low cost. Among various dissimilar bonding processes, the rolled cladding process is widely used in Ti alloys, but has a disadvantage of low bonding strength. Although this problem can be solved through post-heat treatment, the mechanical properties at the bonded interface are deteriorated due to residual stress generated during post-heat treatment. Therefore, in this study, the microstructure change and residual stress trends at the interfaces of Ti/Al cladding materials were studied with increasing post-heat treatment temperature. As a result, compared to the as-rolled specimens, no difference in microstructure was observed in the specimens after postheat treatment at 300, 400, and 500℃. However, a new intermetallic compound layer was formed between Ti and Al when post-heat treatment was performed at a temperature of 600℃ or higher. Then, it was also confirmed that compressive residual stress with a large deviation was formed in Ti due to the difference in thermal expansion coefficient and modulus of elasticity between Ti Grade II and Al 1050.

• Journal of the Korean institute of surface engineering
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• v.34 no.5
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• pp.414-420
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• 2001

A 30-kV plasma immersion ion implantation setup (P $I^3$) has been equipped with a self-developed 6'-magnetron to perform hard coatings with enhanced adhesion by P $I^3$D(P $I^3$ assisted deposition) process. Using ICP source with immersed Ti antenna and reactive magnetron sputtering of Ti target in $N_2$/Ar ambient gas mixture, the TiN films were prepared on Si substrates at different pulse bias and ion-to-atom arrival ratio ( $J_{i}$ $J_{Me}$ ). Prior to TiN film formation the nitrogen implantation was performed followed by deposition of Ti buffer layer under A $r^{+}$ irradiation. Films grown at $J_{i}$ $J_{Me}$ =0.003 and $V_{pulse}$=-20kV showed columnar grain morphology and (200) preferred orientation while those prepared at $J_{i}$ $J_{Me}$ =0.08 and $V_{pulse}$=-5 kV had dense and eqiaxed structure with (111) and (220) main peaks. X-ray diffraction patterns revealed some amount of $Ti_{x}$ $N_{y}$ in the films. The maximum microhardness of $H_{v}$ =35 GN/ $M^2$ was at the pulse bias of -5 kV. The P $I^3$D technique was applied to enhance wear properties of commercial tools of HSS (SKH51) and WC-Co alloy (P30). The specimens were 25-kV PII nitrogen implanted to the dose 4.10$^{17}$ c $m^{-2}$ and then coated with 4-$\mu\textrm{m}$ TiN film on $Ti_{x}$ $N_{y}$ buffer layer. Wear resistance was compared by measuring weight loss under sliding test (6-mm $Al_2$ $O_3$ counter ball, 500-gf applied load). After 30000 cycles at 500 rpm the untreated P30 specimen lost 3.10$^{-4}$ g, and HSS specimens lost 9.10$^{-4}$ g after 40000 cycles while quite zero losses were demonstrated by TiN coated specimens.s.

• Bulletin of the Korean Chemical Society
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• v.25 no.4
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• pp.475-479
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• 2004

$TiO_2$ thin films were grown on Si (100) substrates by atomic layer deposition using $[Ti(OPr^i )_2(dmae)_2]$ and water as precursors. The thickness, chemical composition, crystalline structure, and morphology of the deposited films were investigated by transmission electron microscopy, UV spectrometry, X-ray photoelectron pectroscopy, X-ray diffraction, and atomic force microscopy. The results show that $TiO_2$ ALD using $[Ti(OPr^i )_2(dmae)_2]$ as a precursor is self-controlled at temperatures of 100-300$^{\circ}C$. At the growth temperatures below 300$^{\circ}C$, the surface morphology of the $TiO_2$ films is smooth and uniform. The $TiO_2$ film was grown with a preferred orientation toward the [101] direction at 400$^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.34 no.4
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• pp.373-379
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• 1997

A study on the deposition and characterization of BaTiO3 thin films on MgO-buffered Si(100) substrates by sputtering was conducted. The MgO buffer layers were investigated as a function of deposition temperature. At lower substrate temperature, the MgO layers were not fully crystalline, but a crystallized MgO layer with (001) preferred orientation was obtained at the substrate temperature of $700^{\circ}C$. Partially (00ι) or (h00) textured BaTiO3 films were obtained on Si(100) with the MgO buffer layer grown at 700ι. While, randomly oriented BaTiO3 films with large-scale cracks on the surface were made without the MgO layer. The crystallographic orientation, morphology and electrical properties between the BaTiO3 films on Si with and without the MgO layer were compared using the BaTiO3 film on MgO(100) single crystal substrate as a reference system. Also the favorable role of the MgO layer as a buffer for growing of oriented BaTiO3 films on Si substrates was confirmed.

• Journal of the Korean Ceramic Society
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• v.21 no.3
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• pp.278-282
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• 1984

Barium titanate powder was made by firing the complex hydroxide which had been synthesized with chemical wet process by the medium of $H_2O_2$. This experiment was done as following A mixed solution of $BaCl_2$, $TiCl_4$ and $H_2O_2$ with 1:1:10 mol ratio was prepared. Ammonium hydroxide was added into the mixed solution. In the range of pH 8-10 $BaTiO_3$ complex hydroxide was obtained and treated at room temperature 11$0^{\circ}C$, 20$0^{\circ}C$, 40$0^{\circ}C$ and $600^{\circ}C$. The results obtaiined from this experiment were as follows. At room temperature $BaTiO_3$ complex hydroxide was amorphous. Above 10$0^{\circ}C$ crystalline $BaTiO_3$ was obtained and particle size of $BaTiO_3$ was increased with elevated temperature. So the particle size of BaTiO3 could be controlled by the firing temperature. After treating $BaTiO_3$ complex hydroxide at 10$0^{\circ}C$ the average particle size of $BaTiO_3$ was 0.22$\mu\textrm{m}$.

• Journal of Korean Society for Atmospheric Environment
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• v.6 no.1
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• pp.31-42
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• 1990

In order to suggest an efficient catalyst systems for NOx reduction of flue gases from industrial boilers, $TiO_2$ supported $WO_3-V_2O_5, V_2O_5$ and $WS_2$ catalysts were tested for the performances of NOx reduction at high reactin temperature range (250-500$^\circ$C) using a simulated flue gas system. It was found that while the proposed $WO_3/TiO_2$ and $WO_3-V_2O_5/TiO_2$ catalysts showed a significant high NOx reduction efficiency at about 350-400$^\circ$C, the conventional commercial catalyst of $V_2O_5/TiO_2$ showed a significant drop in NOx reduction efficiency due to the excessive $NH_3$ oxidation. From the measurement of surface acidities of those catalysts, it was found that the acidity are well correlated with the activities of NOx reduction. The reason of high activity of $WO_3$ series catalysts at high reaction temperature seems due to the low value of surface excess oxygen compared with that of $V_2O_5/TiO_2$ seems equivalent to the acid site of that catalyst.

• Korean Journal of Materials Research
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• v.9 no.6
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• pp.577-582
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• 1999

In order to make the electroconductive $Si_3N_4$-TiN composities, the Si-Ti(N) compacts were nitrided at $1450^{\circ}C$ for 20hours, and then they were post-sintered by a gas-pressure-sintering technique at 1TEX>$1950^{\circ}C$ for 3.5 hours. As starting powders, commercial si powder of about $10\mu\textrm{m}$, two types of Ti powders of 100 and 325 mesh, and fine-sized TiN of $2.5\mu\textrm{m}$ powders were used. In the $Si_3N_4$-TiN sintered bodies used Ti powders, the relative density and fracture strength and electrical conductivity are low due to the existence of large amounts of coarse pores. However, in the $Si_3N_4$-TiN composite used TiN powder, the fracture toughness, fracture strength and electrical resistivity were $5.0MPa{\cdot}m^{1/2}$, 624MPa and $1400{\omega}cm$, respectively. The dispersion of TiN particles in the composite inhibited the growth of $Si_3N_4$ in the shape of rod and made strong strain field contrasts at the $Si_3N_4$-TiNinterfaces. It was recognized that microstructural control is required to improve the electrical conductivity and mechanical properties of $Si_3N_4$-TiN composites by dispersing TiN particles homogeneously.

• Journal of the Korean institute of surface engineering
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• v.41 no.5
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• pp.181-188
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• 2008

A.C. impedance properties of HA/Ti compound layer coated Ti-30Ta-($3{\sim}15$)Nb alloys have been studied by electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10 and 15 wt% Nb were manufactured by the vacuum furnace system. And then specimen was homogenized at $1000^{\circ}C$ for 24 hrs. The sample was cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The non-coated and coated morphology of Ti alloy were analyzed by X-ray diffractometer (XRD), energy X-ray dispersive spectroscopy (EDX) and filed emission scanning electron microscope (FE-SEM). The corrosion behaviors were investigated using A.C. impedance test (PARSTAT 2273, USA) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Ti-30Ta-($3{\sim}15\;wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and $\beta$ phase peak was predominantly appeared in the case of increasingly Nb contents. The microstructures of Ti alloy were transformed from needle-like structure to equiaxed structure as Nb content increased. From the analysis of coating surface, HA/Ti composite surface uniformed coating layer with 750 nm thickness. The growth directions of film were (211), (112), (300) and (202) for HA/Ti composite coating on the surface after heat treatment at $550^{\circ}C$, whereas, the growth direction of film was (110) for Ti coating. The polarization resistance ($R_p$) of HA/Ti composite coated Ti-alloys were higher than those of the Ti and HA coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.