• Journal of the Korean Ceramic Society
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• v.37 no.1
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• pp.96-101
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• 2000

Comparative studies on microstructure, and mechanical and anti-oxidation properties between TiN and Ti-Si-N films were performed. The Ti-Si-N films were deposited on high-speed steel and silicon wafer substrates by plasma-assisted chemcial vapor deposition(PACVD) technique. The Si addition to TiN film caused to change the microstructure such as grain size refinement, randomly multi-oriented microstructure, and nano-sized codeposition of silicon nitride in the TiN matrix. The Ti-Si-N film, contains Si content of ∼7 at.%, showed the micro-hardness value of ∼3400 HK, which was higher than the pure TiN film whose hardness was ∼1500HK. The Ti-Si(7 at.%)-N film also showed much improved anti-oxidation properties compared with those of the pure TiN film. These properties were also related to the microstructure of Ti-Si(7 at.%)-N film was formed and retarded further oxidation of the nitridelayer. These properties were also related to the microstructure of Ti-Si(7 at.%)-N film which was characterized by nano-sized precipitates of silicon nitride phase in the TiN matrix and randomly oriented grains.

• Journal of Surface Science and Engineering
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• v.39 no.6
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• pp.245-249
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• 2006

In this study, ternary Ti-Mo-N and new quaternary Ti-Mo-Si-N coatings were synthesized on steel substrates(AISI D2) and Si wafers by a hybrid coating system of arc ion plating (AIP) using Ti target and d.c. magnetron sputtering technique using Mo and Si targets in $N_2/Ar$ gaseous mixture. Ternary Ti-Mo-N coatings were substitutional solid-solution of (Ti, Mo)N and showed maximum hardness of approximately 30 GPa at the Mo content of ${\sim}10$. %. The Ti-Mo-Si-N coating with the Si content of 8.8 at. % was a composite consisting of fine (Ti, Mo)N crystallites and amorphous $Si_3N_4$ phase. The hardness of the Ti-Mo-Si(8.8 at. %)-N coatings exhibited largely increased hardness value of ${\sim}48$ GPa due to the microstructural evolution to the fine composite microstructure and the refinement of (Ti, Mo)N crystallites. The average friction coefficient of the Ti-Mo-Si-N coatings largely decreased with increase of Si content. The microstructures of Ti-Mo-Si-N coatings were investigated with instrumental analyses of XRD, XPS, and HRTEM in this work.

• Korean Journal of Materials Research
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• v.11 no.7
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• pp.580-584
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• 2001

We have investigated the deposition characteristics of Ti-Si-N films obtained by rf magnetron sputtering with ratios of Ti/Si targets in an $Ar/N_2$ gas mixture. The growth rate and stoichiometry dependence of the Ti-Si-N films on the ratio of Ti/Si and $N_2$ flow rate ratio were found to be due to the different nitriding rate of Ti and Si targets. Additionally, their different sputtering yield of nitrified Ti and Si make a reason as well. Lowering Si content in the film favored the formation of crystalline TiN, leading to the low resistivity. Increasing N content led to the Ti-Si-N films having a higher density and compressive stress, suggesting that the N content in the film is one of the most important factors determining the diffusion barrier characteristics. In the current work, the optimum process conditions for the formation of efficient diffusion barrier of Ti-Si-N film has successfully obtained by manipulating the Ti/Si ratio of target and $N_2$ flow rate ratio.

• Journal of Surface Science and Engineering
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• v.35 no.3
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• pp.133-140
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• 2002

The Ti-Si-N coating layers were synthesized on SKD 11 steel substrate by a DC reactive magnetron co-sputtering technique with separate Ti and Si targets. The high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) analyses for the coating layers revealed that microstructure of Ti-Si-N layer was nanocomposite, consisting of nano-sized TiN crystallites surrounded by amorphous $Si_3$$N_4$ phase. The highest hardness value of about 39 GPa was obtained at the Si content of ~11at.%, where the microstructure had fine TiN crystallites (about 5nm in size) dispersed uniformly in amorphous matrix. As the Si content in Ti-Si-N films increased, the TiN crystallites became from aligned to randomly oriented microstructure, finer, and fully penetrated by amorphous phase. Free Si appeared in the layers due to the deficit of nitrogen source at higher Si content. Friction coefficient and wear rate of the Ti-Si-N coating layer significantly decreased with increase of relative humidity. The self-lubricating tribe-layers such as $SiO_2$ or (OH)$Si_2$ seemed to play an important role in the wear behavior of Ti-Si-N film against steel.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2005.10a
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• pp.178-181
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• 2005

Quaternary Ti-Si-C-N coatings were deposited on WC-Co substrates by a hybrid coating system of arc ion plating (AIP) and sputtering techniques using Ti and Si targets, in an $Ar/N_2/CH_4$ gaseous mixture. The crystallinity, bending status, and microstructure of the Ti-Si-C-N coatings were measured by X-ray diffractometer (XRD) and X-ray photoelectron spectroscope (XPS), The micro-hardness of Ti(C,N) and Ti-Si-N coatings were about 30 and 40 GPa, respectively. As the Si was incorporated into Ti(C,N) coatings, the Ti-Si-C-N coatings having Si content of $8.9\;at.\%$ showed the maximum hardness value of about 55 GPa. In this work, the microstructure and mechanical properties of Ti-Si-C-N coatings were systematically investigated.

• 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.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2014.11a
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• pp.304-304
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• 2014

Quaternary Ti-Al-Si-N films were deposited on WC-Co substrates by a hybrid deposition system of arc ion plating (AIP) method for Ti-Al source and DC magnetron sputtering technique for Si incorporation. The synthesized Ti-Al-Si-N films were revealed to be composites of solid-solution (Ti,Al)N crystallites and amorphous $Si_3N_4$ by instrumental analyses. The Si addition in Ti-Al-N films affected the refinement and uniform distribution of crystallites by percolation phenomenon of amorphous silicon nitride, similarly to Si effect in TiN film. As the Si content increased up to about 9 at.%, the hardness of Ti-Al-N film steeply increased from 30 GPa to about 50 GPa. The highest microhardness value (~50 GPa) was obtained from the Ti-Al-Si-N film having the Si content of 9 at.%, the microstructure of which was characterized by a nanocomposite of $nc-(Ti,Al)N/a-Si_3N_4$.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.130-130
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• 2018

산업 발전으로 특수합금들이 발달함에 따라 가공할 수 있는 새로운 절삭공구소재들이 개발되어지고 있다. 또한 공구소재보다 코팅개발이 상대적으로 더욱 효과적이기 때문에 코팅 기술 개발이 활발히 진행되고 있다. 일본에서는 새로운 코팅층 물질 개발보다는 기존의 코팅물질을 조합하거나 개량하여 성능을 향상시키는 추세이다. TiAlSiN 박막은 스퍼터링과 음극 아크 소스를 이용한 hybrid 공정을 이용하여 코팅 후 특성을 평가하였다. Ti-50at.%Al의 조성을 갖는 TiAl 합금 타겟은 음극 아크 소스를 이용하여 코팅하였다. 공정 가스는 Ar과 N2의 혼합 가스를 사용하였으며 공정 압력은 $1.0{\times}10^{-2}Torr$이었다. 음극 아크 소스에 인가된 전류는 70 A이었다. TiAlSiN 박막의 Si 함량을 조절하기 위해서 Si은 스퍼터링으로 코팅하였으며 스퍼터링 소스에 인가되는 전력의 세기를 0.29 kW ~ 1.05 kW까지 변화시켰다. 코팅 공정에 사용된 Si 타겟의 순도는 4N이다. TiAlSiN 박막의 Si 함량은 스퍼터링 전력에 따라 3.4 ~ 14.4at%까지 변화하는 것을 확인하였다. TiAlSiN 코팅층의 경도는 초미소 경도계를 이용하여 측정하였으며, Si 함량이 증가하면 TiAlSiN 박막의 경도도 증가하는 것을 확인할 수 있다. TiAlSiN 박막의 Si 함량이 9.2at.%일 때 3000 Hv 이상의 경도를 보였다. TiAlSiN 코팅층의 Si 함량이 14.4at%로 높아지면 경도가 낮아지는 현상을 보였다. TiAlSiN 박막의 Si 함량이 증가하면 내산화성이 향상되는 현상을 확인할 수 있었다.

• Journal of Surface Science and Engineering
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• v.37 no.3
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• pp.152-157
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• 2004

Ti-Al-N ($Ti_{75}$ $Al_{25}$ N) and Ti-Al-Si-N ($Ti_{69}$ $Al_{23}$ $Si_{8}$N) coatings synthesized by a DC magnetron sputtering technique were studied comparatively with respect to phase characterization and high-temperature oxidation behavior. $Ti_{69}$ $Al_{23}$ $Si_{ 8}$N coating had a nanocomposite microstructure consisting of nanosized(Ti,Al,Si)N crystallites and amorphous $Si_3$$N_4$, with smooth surface morphology. Ti-Al-N coating of which surface $Al_2$$O_3$ layer formed during oxidation suppressed further oxidation. It was sufficiently stable against oxidation up to about $700^{\circ}C$. Ti-Al-Si-N coating showed better oxidation resistance because both surface Ab03 and near-surface $SiO_2$ layers suppressed further oxidation. XRD, GDOES, XPS, and scratch tests were performed.

• Proceedings of the KIEE Conference
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• 1994.07b
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• pp.1223-1225
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• 1994

The properties of $TiN/TiSi_2$ bilayer formed by a rapid thermal anneal ing is investigated when thin $SiO_2$ film exists at the Ti-Si interface. The competitive reaction for the $TiN/TiSi_2$ bilayer occurs above $600^{\circ}C$. The thickness of the $TiSi_2$ layer decreases with increasing $SiO_2$ film thickness while the TiN layer increases at the competitive reaction. The composition of TiN layer is changed to the $TiN_xO_y$ film due to the thin $SiO_2$ layer at the Ti-Si interface while the structure of the TiN and $TiSi_2$ layers was not changed.