• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.354-354
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• 2007

Titanium nitride (TiN) thin films are widely used for hard coatings due to their superior hardness. In this paper, we wanted see how the films properties are changed according to DC power. TiN thin films were deposited by direct current (DC) magnetron sputtering method using TiN compound target on silicon substrates. The films structural properties are examined by X-ray Diffractions (XRD) and tribological properties are measured by nano-indentation, nano-scratch tester, nano-stress tester. Especially in DC power of 150 W, the maximum hardness and the minimum residual stress of TiN film exhibited about 25 GPa and 1 GPa, respectively. And also, the critical load of TiN film prepared by magnetron sputtering method were measured over 30 N.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.195.1-195.1
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• 2013

Cu는 금속 박막재료로서 높은 전기전도성을 지니고 있을 뿐만 아니라 Ag, Al, Pt 등 보다 비용이 저렴하여, 높은 전기전도성을 필요로 하는 박막 재료로써 폭넓게 사용되고 있다. 그러나, 낮은 기계적 특성을 지니고 있어서 interconnect와 같은 작은 단면적의 배선재료로 사용될 경우, 높은 전류밀도에 따른 electromigration 현상에 의하여 hillock 또는 void의 형성 등 박막재료의 변형이 생기게 되어서 전자소자의 수명이 단축된다는 단점이 있다. TiN은 금속재료 못지않은 높은 전기 전도성을 지니고 있을 뿐만 아니라, 금속재료에 비하여 높은 기계적 특성과 녹는점을 지니고 있어 다양한 분야로 사용되고 있다. 본 연구에서는 Cu와 TiN composite 박막을 soda-lime glass위에 증착하여 낮은 비저항 뿐만 아니라 Cu와 비교하여 기계적 특성이 향상된 박막을 제작하고자 하였다. Cu와 TiN composite 박막 증착을 위하여 DC reactive magnetron co-sputtering 장비를 사용하였으며, Cu와 Ti 타겟 power, Ar:N2 유량비(Flow rate)을 변화시켜 Cu와 Ti의 조성비 및 TiN의 결정성을 조절하였고, 이를 통하여 박막의 TiN 조성에 따른 낮은 비저항 값과 순수한 Cu 박막과 비교하여 높은 기계적 특성을 지닌 Cu-TiN 박막을 증착하였다. Cu-TiN composite 박막의 구조 및 조성은 SEM (Scanning Electron Microscope), EDS (Energy Dispersive Spectrometer), XPS (X-ray Photoelectron Spectroscopy)장비를 사용하여 분석하였으며, 전기전도도는 4-point probe를 사용하여 측정하였고, Knoop hardness 측정방법을 사용하여 박막의 기계적 특성을 측정하였다.

• Journal of Advanced Navigation Technology
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• v.17 no.5
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• pp.574-580
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• 2013

In this paper, The process of thin-film coating technology was applied to improve adhesion of the hardness thin film and nitride layer. This thin-film coating technology have formed composite thin-film to gain hardness and toughness used in press mold. The thin-film coating manufacturing technology increased vacuum present in the vacuum chamber and improved the throw ratio of the gun power using physical vapor deposition coating technology. Ti alloys target improved performance and surface material through the development of a composite film coating technology for various precision machining parts.

• Journal of Periodontal and Implant Science
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• v.29 no.1
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• pp.209-231
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• 1999

Even though titanium(Ti) and its alloys are the most used dental implant materials, there are some problems that Ti wears easily and interferes normal osteogenesis due to the metal ions. Ti coated with bioactive ceramics such as hydroxyapatite has also such problems as the exfoliation or resorption of the coated layer, Recent studies on implant materials have been proceeding to improve physical properties of the implant substrate and biocompatibility of the implant surfaces. The purpose of the present study was to examine the physical property and bone tissue compatibility of bioinert nitrides ion plated Ti, Button type specimens(14mm in diameter, 2.32rrun in height) for the abrasion test and cytotoxicity test and thread type implants(3.75mm in diameter, 6mm in length) for the animal experiments were made from Ti(grade 2) and 316LVM stainless steel. Ti specimens were ion plated with TiN, ZrN by the low temperature arc vapor deposition, and the depth profile of the TiN/Ti, ZrN/Ti ion plated surface was examined by Auger Electron Spectroscopy. Three kind of button type specimens .of TiN/Ti, ZrN/Ti and Ti were used for abrasion test, and HEPAlClC7 cells and CCD cells were cultivated for 4 days with the specimens for cytotoxicity test. Thread type implants of TiN/Ti, ZrN/Ti, Ti, 316LVM were implanted on the femur of 6 adult dogs weighing 10kg-13kg. Two dogs were sacrified for histological examination after 45 days and 90 days, and four dogs were sacrified for the removal torque test of the implant') after 90 days. The removal torque force was measured by Autograph (Shimadzu Co., AGS-1000D series, Japan). Abrasion resistance of TiN/Ti was the highest, and that of ZrN/Ti and Ti were followed. The bioinert nitride ion plated Ti had much better abrasion resistance, compared with Ti, In the cytotoxicity test, the number of both cells were increased in all specimens, and there were no significant difference in cytotoxic reaction among all groups (p>0.1), In histological examination, 316LVM showed the soft tissue engagement in interface between the implant and bone, but the other materials after 45 days noted immature new bone formation in the medullary portion along the implant surface, and those after 90 days showed implant support by new bone formation in both the cortical and the medullary portion, The removal torque force of Tilv/Ti showed significantly higher than that of Ti(p(O,05). The difference in removal torque force between TiN/Ti and ZrN/Ti was not significant(p>0.05), and that of 316LVM was lowest among all groups(p<0.05). These results suggest that bioinert nitrides ion plated Ti can resolve the existing problems of Ti and bioactive ceramics, and it may be clinically applicable to human.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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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.

• Proceedings of the KWS Conference
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• 2009.11a
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• pp.72-72
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• 2009

전자부품의 내부접속 및 파워반도체의 다이본딩과 같은 1차실장에는 고온환경에서의 사용과 2차실장에서의 재용융방지를 위해 높은 액상선온도 및 고상선온도를 필요로 하여, Pb-5wt%Sn, Pb-2.5wt%Ag로 대표되는 납성분 85%이상의 고온솔더가 널리 사용되고 있다. 생태계와 인체에 대한 납의 유해성이 보고된 이래, 무연솔더에 대한 연구가 활발히 진행되어 왔으나, Sn-Ag-Cu계로 대표되는 Sn계 합금으로 대체 중인 중온용 솔더와는 달리, 고온용 솔더에 대해서는 대체합금에 대한 연구가 미흡한 실정이다. 대체재의 부재로 인해 기존의 납을 다량함유한 솔더로 1차실장이 지속됨으로서, 2차실장의 무연화에도 불구하고 전자부품 및 기기의 재활용에 큰 어려움을 겪고 있다. 지금까지 고온용 무연솔더로서는 융점에 근거해 Au-(Sn, Ge, Si)계, Bi-Ag계, Zn-(Al, Sn)계의 극히 제한된 합금계만이 보고되어 왔다. Au계 솔더는 현재 플럭스를 사용하지 않는 광학, 디스플레이 분야 등 고부가가치 공정에 사용되고 있으나, 합금가격이 매우 비싸며 가공성이 나빠 대체재료로서는 적합하지 않다. Bi-Ag계 솔더 또한 취성합금으로 와이어 및 박판으로 가공하는데 어려움이 크며, 솔더로서 중요한 특성중 하나인 전기전도도 및 열전도도가 나쁜 편이다. 이에 비해, Zn계 합금은 비교적 낮은 합금가격, 적절한 가공성과 뛰어난 인장강도, 우수한 전기전도도 및 열전도도를 지녀, 고온용솔더 대체재료의 유력한 후보로 생각된다.이전 연구에서, 필자의 연구그룹은 Zn-Sn계 합금을 고온용 무연솔더로서 제안한 바 있다. Zn-Sn계 합금은 충분히 높은 융점과 함께, 금속간화합물이 없는 미세조직, 우수한 기계적 특성, 높은 전기전도도 및 열전도도 등의 장점을 나타내었다. 본 연구에서는 기초합금특성상 고온솔더로서 다양한 장점을 지닌 Zn-30wt%Sn합금을 고온용 솔더의 대표적인 적용의 하나인 다이본딩에 적용하여, 접합부의 강도 및 미세조직, 열피로 신뢰성에 대해 분석을 함으로서 실제 공정에의 적용가능성에 대해 검토하였다. Zn-30wt%Sn을 이용해 Au/TiN(Titanium nitride) 코팅한 Si다이를 AlN-DBC(aluminum nitride-direct bonded copper)기판에 접합한 결과, 양측에 완전히 젖은 기공이 없는 양호한 다이접합부를 얻었으며, 솔더내부에는 금속간화합물을 형성하지 않았다. Si다이와의 계면에는 TiN만이 존재하였으며, Cu와의 계면에는 Cu로부터 $Cu_5Zn_8,\;CuZn_5$의 반응층을 형성하였다. 온도사이클시험을 통한 열피로특성평가에서, Zn-30wt%Sn를 이용한 다이접합부는 1500사이클 지점에서 Cu와 Cu-Zn금속간화합물의 사이에서 피로균열이 형성되며, 접합강도가 크게 감소하였다. 열피로특성 향상을 위해 Cu표면에 TiN코팅을 하여 Zn-30wt%Sn 솔더로 다이접합한 결과, Si다이와 기판 양측에 TiN만으로 구성된 계면을 형성하였으며, TEM관찰을 통해 Zn-30wt%Sn과 극히 미세한 접합계면이 형성하고 있음을 확인하였다. Zn-wt%30Sn솔더와 TiN층의 병용으로 2000사이클까지 미세조직의 변화 및 강도저하가 없는 극히 안정된 고신뢰성의 다이접합부를 얻을 수가 있었다.

• Journal of the Korean Ceramic Society
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• v.31 no.12
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• pp.1577-1587
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• 1994

TiO2 thin films with the substitution of oxygen with nitrogen were deposited on silicon substrate by metalorganic chemical vapor deposition (MOCVD) using Ti(OCH(CH3)2)4 (titanium tetraisopropoxide, TTIP) and N2O as source materials. X-ray diffraction (XRD) results indicated that the crystal structure of the deposited thin films was anatase TiO2 with only (101) plane observed at the deposition temperatures of 36$0^{\circ}C$ and 38$0^{\circ}C$, and with (101) and (200) plane at above 40$0^{\circ}C$. Raman spectroscopic results indicated that the crystal structure was anatase TiO2 in accordance with the XRD results without any rutile, fcc TiN, or hcp TiN structure. No fundamental difference was observed with temperature increase, but the peak intensity at 194.5 cm-1 increased with strong intensity at 143.0 cm-1 for all samples. The crystalline size of the films varied from 49.2 nm to 63.9 nm with increasing temperature as determined by slow-scan XRD experiments. The refractive index of the films increased from 2.40 to 2.55 as temperature increased. X-ray photoelectron spectroscopy (XPS) study showed only Ti 2s, Ti 2p, C 1s, O 1s and O 2s peaks at the surface of the film. The composition of the surface was estimated to be TiO1.98 from the quatitative analysis. In the bulk of the film Ti 2s, Ti 2p, O 1s, O 2s, N 1s and N 2s were detected, and Ti-N bonding was observed due to the substitution of oxygen with nitrogen. A satellite structure was observed in the Ti 2p due to the Ti-N bonding, and the composition of titanium nitride was determined to be about TiN1.0 from the position of the binding energy of Ti-N 2p3/2 and the quatitative analysis. The spectrum of Ti 2p energy level could be the sum of a 4, 5, or 6 Gaussian curve reconstruction, and the case of the sum of the 6 Gaussian curve reconstruction was physically most meaningful. From the results of Auger electron spectroscopy (AES), it was known that the composition was not varied significantly throughout the whole thickness of the film, and silicon oxide was not observed at the interface between the film and the substrate. The composition of the film was possible (TiO2)1-x.(TiN)x or TiO2-2xNx and in this experimental condition x was found to be about 0.21-0.16.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.74-74
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• 2009

Titanium nitride has been used as hardmask for semiconductor process, capacitor of MIM type and diffusion barrier of DRAM, due to it's low resistivity, thermodynamic stability and diffusion coefficient. Characteristics of the TiN film are high intensity and chemical stability. The TiN film also has compatibility with high-k material. This study is an experimental test for better condition of TiN film etching process. The etch rate of TiN film was investigated about etching in $BCl_3/Ar/O_2$ plasma using the inductively coupled plasma (ICP) etching system. The base condition were 4 sccm $BCl_3$ /16 sccm Ar mixed gas and 500 W the RF power, -50 V the DC bias voltage, 10 mTorr the chamber pressure and $40\;^{\circ}C$ the substrate temperature. We added $O_2$ gas to give affect etch rate because $O_2$ reacts with photoresist easily. We had changed $O_2$ gas flow rate from 2 sccm to 8 sccm, the RF power from 500 W to 800 W, the DC bias voltage from -50 V to -200 V, the chamber pressure from 5 mTorr to 20 mTorr and the substrate temperature from $20\;^{\circ}C$ to $80\;^{\circ}C$.

• Journal of the Korean Society for Heat Treatment
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• v.18 no.5
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• pp.281-287
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• 2005

Titanium aluminium nitride((TiAl)N) film is anticipated as an advanced coating film with wear resistance used for drills, bites etc. and with corrosion resistance at a high temperature. In this study, (TiAl)N thin films were deposited both at room temperature and at elevated substrate temperatures of 573 to 773 K by using a two-facing-targets type DC sputtering system in a mixture Ar and $N_2$ gases. Atomic compositions of the binary Ti-Al alloy target is Al-rich (25Ti-75Al (atm%)). Process parameters such as precursor volume %, substrate temperature and Ar/$N_2$ gas ratio were optimized. The crystallization processes and phase transformations of (TiAl)N thin films were investigated by X-ray diffraction, field-emission scanning electron microscopy. The microhardness of (TiAl)N thin films were measured by a dynamic hardness tester. The films obtained with Ar/$N_2$ gas ratio of 1:3 and at 673 K substrate temperature showed the highest microhardness of $H_v$ 810. The crystallized and phase transformations of (TiAl)N thin films were $Ti_2AlN+AlN{\rightarrow}TiN+AlN$ for Ar/$N_2$ gas ratio of 1:3, $Ti_2AlN+AlN{\rightarrow}TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 1:1 and $TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN{\rightarrow}Ti_2AlN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 3:1. The above results are discussed in terms of crystallized phases and microhardness.

• Journal of the Korean Society for Heat Treatment
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• v.23 no.1
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• pp.29-33
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• 2010

Titanium nitride (TiN) films were deposited on the polycarbonate substrate by using radio frequency (RF) magnetron sputtering without intentional substrate heating. After deposition, the films were bombarded with intense electron beam for 20 minutes. The intense electron irradiation impacts on the crystalline, hardness and surface roughness of the TiN films. The films irradiated with an electron beam of 300 eV show the small grains on the surface, while as deposited TiN films did not showany grains on the surface. Also the surface harness evaluated with micro indenter was increased up to 18 Gpa at electron energy of 900 eV after electron beam irradiation. In addition, surface root mean square (RMS) roughness of the films irradiated with intense electron beam affected strongly. The films irradiated by electron beam with 900 eV have the lowest roughness of 1.2 nm in this study.