• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.132-132
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• 2016

기계 가공품의 정밀화, 경량화 요구로 난색재로 분류되는 비철분야 및 복합재 가공용 공구개발에 대한 수요가 급증하고 있으나, 기존 난삭재 가공 시 절삭공구의 마모가 빠르고, 상대재의 융착 불량 등이 공구 수명 감소의 주요 영향으로 보고된다. 상기문제를 해결하기 위해 절삭가공 공정 중 과다한 절삭유의 사용에 따른 가공비용, 에너지소모 증가, 환경오염 등으로 절삭유의 최소화 또는 절삭유를 사용하지 않는 표면처리기술등의 친환경 가공기술의 개발이 필요하다. 내융착 및 내마모 특성 향상을 위한 표면코팅 방법으로 수소가 포함되지 않은 고경도 비정질 카본 (ta-C)이 있으나, ta-C 코팅 막은 경도 30 - 80 GPa, 잔류응력 3 - 10 GPa 범위로 일반 경질 코팅 막 (AlTiN, TiSiCrN : 평균 3 GPa)에 비해 높고 산업적 활용이 가능한 0.5 - 1.5 um 두께 수준의 후막화가 힘들어 매우 우수한 절삭공구용 코팅 막 특성에도 불구하고 적용사례가 매우 적다. 따라서, 본 연구에서는 아크플라즈마 방식 (Filtered Cathode Vacuum Arc Plasma, FCVA)을 활용한 고경도/무수소 카본 코팅 막을 후막형태로 증착하여 비철금속가공용 절삭 공구류의 수명향상 기법을 제시하고자 한다. ta-C 코팅 막의 기초 공정개발 단계에서는 바이어스 전압, 공정시간을 달리하여 ta-C 코팅 막의 기계적 물성(경도: $50{\pm}3GPa$, 잔류응력: $6{\pm}1GPa$, 밀착력: 30N 이상 및 트라이볼로지 특성: 마찰계수 0.1 이하, 마멸량: $1.85{\times}10-14mm^3$)을 확보하여 절삭공구로의 공정실용화 적용검토를 실시하였다. ta-C 코팅 막은 (1) WC 공구 및 기존 상용품인 (2) TiAlN/TiN/WC 구조에 대해 증착을 실시하였으며 코팅 막의 두께 변화에 따른 실제 절삭환경에서의 내수명 관측을 진행하였다. 시험결과, ta-C/WC의 단일막 구조인 절삭공구의 경우, 실제 절삭환경에서 쉽게 박리가 발생하여 코팅 막으로서의 효과를 나타내지 못하였다. 이는, 기초 공정개발 단계에서의 밀착력 기준이 실제 환경과 부합하지 않는 것을 의미하며 추후 공정개선을 통해 극복하고자 한다. 반면에, 상용품인 (2) TiAlN/TiN/WC 구조의 절삭공구 대비 ta-C/TiAlN/TiN/WC 구조에서 내수명 증가는 약 2.5배 (기존 300회, 코팅 후 800회)로 증가하였으며 ta-C 코팅 막의 두께가 $0.6-0.8{\mu}m$일 때 최대치를 취한 후 감소하였다. 이를 통해, 절삭공구로의 ta-C 코팅 막 효과는 최외각 층의 두께 범위와 모재 강도보강을 할 수 있는 적절한 중간층 막 (TiN/TiAlN 층)이 혼합되어 나타난 것으로 사료되며 현재 산업계로의 적용을 위한 대량생산용 코팅장비의 개발 및 비용절감을 위한 공정개발이 진행 중이다.

• Journal of the Korean Ceramic Society
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• v.34 no.2
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• pp.202-208
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• 1997

Bi-layered SrBi2Ta2O9(SBT) films were deposited on Pt/Ti/SiO2/Si sibstrates by rf magnetron sputt-ering at room temperature and then were annealed at 75$0^{\circ}C$, 80$0^{\circ}C$ and 85$0^{\circ}C$ for 1 hour in oxygen at-mosphere. The film composition of SrBi2Ta2O9 was obtained after depositing at room temperature and annealing at 80$0^{\circ}C$. Excess 20mole% Bi2O3 and 30 mole% SrCO3 were added to the target to compensate for the lack of Bi and Sr in SBT film. 200 nm thick SBT film exhibited and dense microstructure, adielectric constant of 210, and a dissipation factor of 0.05 at 1 MHz frequency. The films exhibited Curie temperature of 32$0^{\circ}C$ and a dielectric constant of 314 at that temperature under 100 kHz frequency. The remanent polarization(2Pr) and the coercive field(2Ec) of the SBT films were 9.1 $\mu$C/$\textrm{cm}^2$ and 85 kV/cm at an applied voltage of 3V, resspectively and the SBT film showed a fatigue-free characteristics up to 1010 cy-cles under 5V bipolar pulse. The leakage current density of the SBT film was about 7$\times$10-7A/$\textrm{cm}^2$ at 150 kV/cm. Fatigue-free SBT films prepared by rf magnetron sputtering can be suitable for application to non-volatile memory device.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.23-23
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• 2018

In this study, new titanium alloys were prepared by adding elements such as tantalum (Ta), zirconium (Zr) and the like to complement the biological, chemical and mechanical properties of titanium alloys. The Ti-40Ta-xZr ternary alloy was formed on the basis of Ti-40Ta alloy with the contents of Zr in the contents of 0, 3, 7 and 15 wt. %. Plasma electrolytic oxidation (PEO), which combines high-voltage sparks and electrochemical oxidation, is a novel method to form ceramic coatings on light metals such as Ti and its alloys. These oxide film produced by the electrochemical surface treatment is a thick and uniform porous form. It is also composed of hydroxyapatite and calcium phosphate-based phases, so it has the characteristics of bone inorganic, non-toxic and very high bioactivity and biocompatibility. Ti-40Ta-xZr alloys were homogenized in an Ar atmosphere at $1050^{\circ}C$ for 1 hour and then quenched in ice water. The electrochemical oxide film was applied by using a power supply of 280 V for 3 minutes in 0.15 M calcium acetate monohydrate ($Ca(CH_3COO)_2{\cdot}H_2O$) and 0.02 M calcium glycerophosphate ($C_3H_7CaO_6P$) electrolyte. A small amount of 0.0075M zinc acetate and magnesium acetate were added to the electrolyte to enhance the bioactivity. The mechanical properties of the coated surface of Ti-40Ta-xZr alloys were evaluated by Vickers hardness, roughness test, and elastic modulus using nano-indentation, and the surface wettability was evaluated by measuring the contact angle of the coated surface. In addition, cell activation and differentiation were examined by cell culture of HEK 293 (Human embryonic kidney 293) cell proliferation. Surface properties of the alloys were analyzed by scanning electron microscopy(FE-SEM), EDS, and X-ray diffraction analysis (XRD).

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07a
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• pp.350-353
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• 2002

High voltage SiC Schottky barrier diodes with field plate structure have been fabricated and characterized. N-type 4H-SiC wafer with an epilayer of ∼10$\^$15/㎤ doping level was used as a starting material. Various Schottky metals such as Ni, Pt, Ta, Ti were sputtered and thermally-evaporated on the low-doped epilayer. Ohmic contact was formed at the backside of the SiC wafer by annealing at 950$^{\circ}C$ for 90 sec in argon using rapid thermal annealer. Field oxide of 550${\AA}$ in thickness was formed by a wet oxidation process at l150$^{\circ}C$ for 3h and subsequently heat-treated at l150$^{\circ}C$ for 30 min in argon for improving oxide quality. The turn-on voltages of the Ni/4H-SiC Schottky diode was 1.6V which was much higher than those of Pt(1.0V), Ta(0.7V) and Ti(0.7). The voltage drop was measured at the current density of 100A/$\textrm{cm}^2$ showing 2.1V for Ni Schottky diode, 1.45V for Pt 1.35V, for Ta, and 1.25V for Ti, respectively. The maximum reverse breakdown voltage was measured 1100V in the file plated Schottky diodes with 101an thick epilayer.

• Journal of the Korean Ceramic Society
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• v.40 no.1
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• pp.52-61
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• 2003

$SrBi_2Ta_2O_9(SBT)$and$ZrO_2$thin films for MFIS structure(Metal-Ferroelectric-Insulator-Semiconductor) were deposited by RF magnetron sputtering method. In order to investigate the effect of heat treatment of insulator layers and MFIS structure, the insulator layers were heat treated from $550^{circ}C;to; 850^{\circ}C$in conventional furnace or RTA furnace under$O_2$and Ar ambient, respectively. After then, C-V characteristics and leakage current were measured. The capacitor with 20 nm thick $ZrO_2$layer treated at RTA$750^{circ}C;in;O_2$ atmosphere had the largest memory window. The C-V and leakage current characteristics of the$Pt/SBT(260nm)/ZrO_2(20nm)/Si$structure were better than those of$Pt/SBT(260nm)/Si$ structure. These results showed that$ZrO_2$films took a role of buffer layer effectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2004.07b
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• pp.965-968
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• 2004

Effective transverse Piezoelectric Coefficients $(e_{31,f})$ of thick PZT $(Pb(Zr_{0.52}Ti{0.48}Ti_{0.48})O_3)$ films on $SiN_x/Si$ substrates were measured with PZT thicknesses and top electrode dimensions. $e_{31,f}$ is one of important Parameters characterizing Piezoelectricity of PZT films. Thick PZT films have been used as various sensors and actuators because of their high driving force and high breakdown voltage. Thick PZT films were fabricated on Pt/Ta/$SiN_x$/Si substrates using sol-gel method. Thicknesses of PZT films were $1{\mu}m$ and $1.8{\mu}m$. $|e_{31,f}|$ values of $1.8{\mu}m$-thick-PZT films were higher than those of $1{\mu}$-thick-PZT films. Maximum $|e_{31,f}|$ of $1.8{\mu}$-thick-PZT films was about $50^{\circ}C/m^2$.

• Korean Journal of Crystallography
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• v.11 no.2
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• pp.95-101
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• 2000

Ferroelectric SrBi2Ta2O9 (SBT) thin films of Pt/Ti/SiO2 electrode were fabricated using a sintered SBT target with various Bi2O3 content by rf magnetron sputtering. Good hysteresis loop characteristics were observed in the SBT thin films deposited with 50mol% excess Bi target. SBT thin films crystallized from 650℃ however, good hysteresis loop can be obtained in the film annealed above 700℃. pt/TiO2/SiO2 and Pt/SiO2 electrodes were also used to investigate the Pt electrode dependence of SBT thin films. SBT thin films showed random oriented polycrystalline structure and similar morphology regardless of electrodes with quite different surface morphology. A 0.2㎛ thick SBT film annealed at 750℃ exhibited the remanent polarization (2Pr) of μC/㎠ and coercive voltage(Vc) of 1V at an applied voltage of 5V.

• Journal of the Korean Magnetics Society
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• v.12 no.6
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• pp.212-217
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• 2002

The pseudo spin valve with a structure of Tl/CoFe(t $\AA$)/Cu(30 $\AA$)/NiFe(50 $\AA$)/Ta, showing giant magnetoresistance properties by utilizing coercivity difference between only two soft ferromagnetic layers were produced by d.c UHV magnetron sputtering system. In pseudo spin valve Ta/CoFe/Cu/NiFe/Ta, the magnetic and magnetoresistance properties with change of CoFe thickness were investigated. When the thickness of CoFe was 60 $\AA$, a typical MR curve of pseudo spin valve structure was obtained, showing MR ratio of 3.8 cio and the coercivity difference of 27.4 Oe with a sharp change of hard layer switching. When the CoFe thickness was varied from 20 to 100 $\AA$, coercivity difference between two layers was increased to 40 $\AA$. and decreased to 100 $\AA$ gradually. It is thought the change in coercivity of hard layer was due to the crystallinity and magnetostriction of thin CoFe layer. In order to improve the MR property in CoFe/Cu/NiFe trier layer structure, CoFe layer with change of 2-20 $\AA$ thick was inserted between Cu and NiFe. When the thickness of CoFe was 10 $\AA$, MR ratio was 6.7％, showing excellent MR property. This indicates 50 ％ higher than that of CoFe/Cu/NiFe pseudo spin valve.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.239-240
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• 2008

As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

• Food Science and Preservation
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• v.20 no.2
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• pp.151-157
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• 2013

This study was conducted to investigate the effect of mature stages on quality of Rafito tomatoes (Lycopersicon esculentum Mill.) during storage at low temperature. Tomatoes grown in greenhouse were harvested at three different mature stages (turning, pink, and red), packaged with a 30-${\mu}m$-thick polyethylene film, and then stored at 5 and $10^{\circ}C$, respectively. The changes in firmness, soluble solids content (SSC), titratable acidity (TA), colour, lycopene content, decay, and chilling injury were measured on a weekly basis. After three weeks of storage, chilling injury and decay were found to have individually occurred at 5 and $10^{\circ}C$, respectively. As there was little change in quality at $5^{\circ}C$, it was concluded that red tomatoes could maintain their good quality for two weeks. The normal postharvest ripening was inhibited in the turning and pink tomatoes during storage at $5^{\circ}C$. The turning and pink tomatoes showed improved quality after two-week storage at $10^{\circ}C$. In particular, the turning fruits showed the highest firmness throughout the storage period. Furthermore, the red colour, SSC/TA, and lycopene content of the turning fruits reached the same levels as with the red fruits after two-week storage at $10^{\circ}C$. These results suggest that red tomatoes should be stored at $5^{\circ}C$ to inhibit decay, and that the optimum temperature for early-harvested tomato (turning and pink) is $10^{\circ}C$ for the ripening process after harvest.