• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.131-131
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• 2018

최근 절삭공구산업은 자동차, 항공기, IT, 선박, 에너지 등 첨단산업의 증가로 인해 CGI, CFRP, 내열합금 등 난삭재의 수요가 증가하고 있다. 난삭재는 고내열, 고경도, 초경량 같은 특성을 지니며 우수한 기계적 물성을 갖지만 가공의 어려움이 있어 산업에 적용하는데 한계가 있다. 이러한 한계를 극복하기 위해 개발된 가공기술 중 하드 코팅은 공구코팅비용 대비 공구의 표면경도와 수명을 효율적으로 향상시킬 수 있다고 알려져 있다. 대표적인 하드코팅으로는 AlN계, TiN계 코팅이 있다. 이러한 코팅의 경우 높은 기계적 물성과 우수한 내마모성으로 인해 절삭공구의 성능을 향상시킬 수 있기 때문에, 많은 연구가 진행되고 있으며 절삭공구산업에서 각광받고 있다. 기존 선행연구 결과에 따르면 질화물 코팅의 우수한 물성은 질화물(Nitride) 생성 및 질화 공정에 의한 코팅층의 고밀도화에 의해 나타난다고 알려져 있다. 그 중에서 AlCrN coating은 우수한 내마모성 및 향상된 고온경도를 갖고 있다. AlCrN based coating에 미량의 원소를 첨가하여 기존 AlCrN coating의 기계적 특성을 더욱 향상 시킨 coating은 일반적인 고성능 코팅 대비 공구수명이 길다고 알려져 있으며, 전반적으로 우수한 특성에 의해 전 세계적으로 습식 및 건식 기계 가공 용도로 사용되고 있다. 본 연구에서는 AlCrN based coating에 미량의 원소를 첨가한 coating의 우수한 기계적 특성의 원인을 규명하기 위해 텅스텐카바이드(WC) 기판 위에 아크 이온 플레이팅 장비를 이용하여 AlCrN based coating을 증착 시킨 sample을 분석하였다. 결정구조 및 상 분석을 위해 X선 회절분석(XRD)을 실시하였으며, 미세 구조를 분석하기 위해 전계방출형 주사전자현미경(FE-SEM), 투과 전자현미경(TEM) 분석을 실시하였다. 또한 코팅층의 화학적 성분 분석을 위해 EDX분석을 실시하였으며 기계적 특성 평가를 위해 나노압입시험(Nano-indentation test)을 진행하였다.

• Journal of the Korean Vacuum Society
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• v.17 no.6
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• pp.528-537
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• 2008

60 nm and 20 nm thick hydrogenated amorphous silicon(a-Si:H) layers were deposited on 200 nm $SiO_2$/single-Si substrates by inductively coupled plasma chemical vapor deposition(ICP-CVD). Subsequently, 30 nm-Ni layers were deposited by an e-beam evaporator. Finally, 30 nm-Ni/(60 nm and 20 nm) a-Si:H/200 nm-$SiO_2$/single-Si structures were prepared. The prepared samples were annealed by rapid thermal annealing(RTA) from $200^{\circ}C$ to $500^{\circ}C$ in $50^{\circ}C$ increments for 40 sec. A four-point tester, high resolution X-ray diffraction(HRXRD), field emission scanning electron microscopy(FE-SEM), transmission electron microscopy(TEM), and scanning probe microscopy(SPM) were used to examine the sheet resistance, phase transformation, in-plane microstructure, cross-sectional microstructure, and surface roughness, respectively. The nickel silicide from the 60 nm a-Si:H substrate showed low sheet resistance from $400^{\circ}C$ which is compatible for low temperature processing. The nickel silicide from 20 nm a-Si:H substrate showed low resistance from $300^{\circ}C$. Through HRXRD analysis, the phase transformation occurred with silicidation temperature without a-Si:H layer thickness dependence. With the result of FE-SEM and TEM, the nickel silicides from 60 nm a-Si:H substrate showed the microstructure of 60 nm-thick silicide layers with the residual silicon regime, while the ones from 20 nm a-Si:H formed 20 nm-thick uniform silicide layers. In case of SPM, the RMS value of nickel silicide layers increased as the silicidation temperature increased. Especially, the nickel silicide from 20 nm a-Si:H substrate showed the lowest RMS value of 0.75 at $300^{\circ}C$.

• Korean Journal of Materials Research
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• v.21 no.2
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• pp.111-114
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• 2011

As a growth-template of ZnO nanorods (NR), a hexagonal $\beta-Ni(OH)_2$ nanosheet (NS) was synthesized with the low temperature hydrothermal process and its microstructure was investigated using a high resolution scanning electron microscope and transmission electron microscope. Zinc nitrate hexahydrate was hydrolyzed by hexamethylenetetramine with the same mole ratio and various temperatures, growth times and total concentrations. The optimum hydrothermal processing condition for the best crystallinity of hexagonal $\beta-Ni(OH)_2$ NS was determined to be with 3.5 mM at $95^{\circ}C$ for 2 h. The prepared $Ni(OH)_2$ NSs were two dimensionally arrayed on a substrate using an air-water interface tapping method, and the quality of the array was evaluated using an X-ray diffractometer. Because of the similarity of the lattice parameter of the (0001) plane between ZnO (wurzite a = 0.325 nm, c = 0.521 nm) and hexagonal $\beta-Ni(OH)_2$ (brucite a = 0.313 nm, c = 0.461 nm) on the synthesized hexagonal $\beta-Ni(OH)_2$ NS, ZnO NRs were successfully grown without seeds. At 35 mM of divalent Zn ion, the entire hexagonal $\beta-Ni(OH)_2$ NSs were covered with ZnO NRs, and this result implies the possibility that ZnO NR can be grown epitaxially on hexagonal $\beta-Ni(OH)_2$ NS by a soluble process. After the thermal annealing process, $\beta-Ni(OH)_2$ changed into NiO, which has the property of a p-type semiconductor, and then ZnO and NiO formed a p-n junction for a large area light emitting diode.

• Journal of Welding and Joining
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• v.33 no.5
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• pp.26-30
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• 2015

Hastelloy X in this study was applied in jet engine F-15 air fighter as shroud to isolate the engine from outer skin. After 15 years operation at elevated temperature the mechanical properties decreased gradually due to the precipitation of continues second phases in the grain boundaries and precipitated inside the grain. The crack happened at the edge of the shroud due to the thermal and mechanical stress from jet engine. Selective TEM analysis found that the grain boundaries consist of $M_{23}C_6$ carbide, $M_6$ Ccarbide and small percentage of sigma(${\sigma}$) phase. Furthermore, it was confirmed the nano size of ${\sigma}$ and miu (${\mu}$) phase inside the grain. In this study, it was investigated the microstructure of the degraded shroud component and HAZ of repair welded shroud. In the HAZ, it was observed the dissolution of the $M_{23}C_6$ carbides and smaller precipitates, the migration of the undissolved larger $M_{23}C_6$ carbide and $M_6$ Ccarbide. It is also observed the liquation due to the simply melt of the segregated precipitates in the grain boundaries. Interestingly, the segregated second phases which simply melt in the grain boundaries more easily happened at higher heat input welding condition. High temperature tensile test was done at $300^{\circ}C$, $700^{\circ}C$ and $900^{\circ}C$. It was obtained that the toughness of welded sample is lower compare to the non-welded sample. The solution heat treatment at $1170^{\circ}C$ for 5 minutes was suggested to obtain a better mechanical properties of the shroud. The high cycle fatigue number of the repair welded shroud shows a much lower compare to the shroud. In addition, the high cycle fatigue number at room temperature after solution heat treatment was almost double compare to the before solution heat treatment under 420-500MPa stress amplitude. However, the high cycle fatigue number of repaired welded sample was shown a much lower compare to the non- welded shroud and solution treated shroud. One of the main reasons to decrease the tensile strength and the high cycle fatigue properties of the repair welded shroud is the formation of the liquid phase in HAZ.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.3
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• pp.135-141
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• 2013

Mechanical alloying was carried out to produce $CrSi_2$ thermoelectric compound using a mixture of elemental $Cr_{33}Si_{67}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of $CrSi_2$ compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry measurement. $CrSi_2$ intermetallic compound with a grain size of 70 nm could be obtained by MA of $Cr_{33}Si_{67}$ powders for 70 hours and subsequently annealed at $650^{\circ}C$. Consolidation of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $600{\sim}1000^{\circ}C$ under 60 MPa. The shrinkage of MA samples during SPS consolidation process increased gradually with increasing temperature up to $1000^{\circ}C$ and relatively significant at about $600^{\circ}C$. We tend to believe that these behaviors are deeply related to form a $CrSi_2$ compound during heating process, as can be realized from the DSC measurement. Electrical conductivity and Seebeck coefficient of sintered bodies were measured up to $900^{\circ}C$. Seebeck coefficient and power factor of $Cr_{33}Si_{67}$ compact prepared by MA and SPS at $1000^{\circ}C$ showed the maximum value of $125{\mu}V/K$ at $400^{\circ}C$ and $4.3{\times}10^{-4}W/mK^2$ at $350^{\circ}C$, respectively.

• Journal of the Microelectronics and Packaging Society
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• v.13 no.4
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• pp.27-36
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• 2006

We fabricated thermally evaporated 10 nm-Ni/(poly)Si, 10 nm-Ni/l nm-Ir/(poly)Si and 10 nm-Ni/l nm-Pt/(poly)Si films to investigate the thermal stability of nickel monosilicides at the elevated temperatures by rapid annealing them at the temperatures of $300{\sim}1200^{\circ}C$ for 40 seconds. Silicides of 50 nm-thick were formed on top of both the single crystal silicon actives and the polycrystalline silicon gates. A four-point tester was used to examine sheet resistance. A scanning electron microscope and field ion beam were employed for thickness and microstructure evolution characterization. An X-ray diffractometer and an Auger depth profiler were used for phase and composition analysis, respectively. Nickel silicides with platinum have no effect on widening the NiSi stabilization temperature region. Nickel silicides with iridium farmed on single crystal silicon showed a low resistance up to $1200^{\circ}C$ while the ones formed on polycrystalline silicon substrate showed low resistance up to $850^{\circ}C$. The grain boundary diffusion and agglomeration of silicides lowered the NiSi stable temperature with polycrystalline silicon substrates. Our result implies that our newly proposed Ir added NiSi process may widen the thermal process window for nano CMOS process.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.25 no.4
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• pp.127-134
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• 2015

Aluminum nitride (AlN) single crystals have attracted much attention for a next-generation semiconductor application because of wide bandgap (6.2 eV), high thermal conductivity ($285W/m{\cdot}K$), high electrical resistivity (${\geq}10^{14}{\Omega}{\cdot}cm$), and high mechanical strength. The bulk AlN single crystals or thin film templates have been mainly grown by PVT (sublimation) method, flux method, solution growth method, and hydride vapor phase epitaxy (HVPE) method. Since AlN suffers difficulty in commercialization due to the defects that occur during single crystal growth, crystalline quality improvement via defects analyses is necessary. Etch pit density (EPD) analysis showed that the growth misorientations and the defects in the AlN surface exist. Transmission electron microscopy (TEM) and electron back-scattered diffraction (EBSD) analyses were employed to investigate the overall crystalline quality and various kinds of defects. TEM studies show that the morphology of the AlN is clearly influenced by stacking fault, dislocation, second phase, etc. In addition EBSD analysis also showed that the zinc blende polymorph of AlN exists as a growth defects resulting in dislocation initiator.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.7 no.6
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• pp.1056-1063
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• 2006

Thermal evaporated 10 nm-Ni/l nm-Ir/(or polycrystalline)p-Si(100) and 10 nm-$Ni_{50}Co_{50}$/(or polycrystalline)p-Si(100) films were thermally annealed using rapid thermal annealing fur 40 sec at $300{\sim}1200^{\circ}C$. The annealed bilayer structure developed into Ni(Ir or Co)Si and resulting changes in sheet resistance, microstructure, phase and composition were investigated using a four-point probe, a scanning electron microscopy, a field ion beam, an X-ray diffractometer and an Auger electron spectroscope. The final thickness of Ir- and Co-inserted nickel silicides on single crystal silicon was approximately 20$\sim$40 nm and maintained its sheet resistance below 20 $\Omega$/sq. after the silicidation annealing at $1000^{\circ}C$. The ones on polysilicon had thickness of 20$\sim$55 nm and remained low resistance up to $850^{\circ}C$. A possible reason fur the improved thermal stability of the silicides formed on single crystal silicon substrate is the role of Ir and Co in preventing $NiSi_2$ transformation. Ir and Co also improved thermal stability of silicides formed on polysilicon substrate, but this enhancement was lessened due to the formation of high resistant phases and also a result of silicon mixing during high temperature diffusion. Ir-inserted nickel silicides showed surface roughness below 3 nm, which is appropriate for nano process. In conclusion, the proposed Ir- and Co- inserted nickel silicides may be superior over the conventional nickel monosilicides due to improved thermal stability.

• Journal of the Korean institute of surface engineering
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• v.38 no.2
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• pp.65-68
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• 2005

The effect of crystal orientation and microstructure on the mechanical properties of $TaN_x$ was investigated. $TaN_x$ films were grown on $SiO_2$ substrates by ultrahigh vacuum unbalanced magnetron sputter deposition in mixed $Ar/N_2$ discharges at 20 mTorr (2.67 Pa) and at $350^{\circ}C$. Unlike the Ti-N system, in which TiN is the terminal phase, a large number of N-rich phases in the Ta-N system could lead to layers which had nano-sized lamella structure of coherent cubic and hexagonal phases, with a correct choice of nitrogen fraction in the sputtering mixture and ion irradiation energy during growth. The preferred orientations and the micro-structure of $TaN_x$ layers were controlled by varing incident ion energy $E_i\;(=30eV\~50eV)$ and nitrogen fractions $f_{N2}\;(=0.1\~0.15)$. $TaN_x$ layers were grown on (0002)-Ti underlayer as a crystallographic template in order to relieve the stress on the films. The structure of the $TaN_x$ film transformed from Bl-NaCl $\delta-TaN_x$ to lamellar structured Bl-NaCl $\delta-TaN_x$ + hexagonal $\varepsilon-TaN_x$ or Bl-NaCl $\delta-TaN_x$ + hexagonal $\gamma-TaN_x$ with increasing the ion energy at the same nitrogen fraction $f_{N2}$. The hardness of the films also increased by the structural change. At the nitrogen fraction of $0.1\~0.125$, the structure of the $TaN_x$ films was changed from $\delta-TaN_x\;+\;\varepsilon-TaN_x\;to\;\delta-TaN_x\;+\;\gamma-TaN_x$ with increasing the ion energy. However, at the nitrogen fraction of 0.15 the film structure did not change from $\delta-TaN_x\;+\;\varepsilon-TaN_x$ over the whole range of the applied ion energy. The hardness increased significantly from 21.1 GPa to 45.5 GPa with increasing the ion energy.

• Korean Journal of Metals and Materials
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• v.47 no.5
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• pp.322-329
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• 2009

60 nm- and 20 nm-thick hydrogenated amorphous silicon (a-Si:H) layers were deposited on 200 nm $SiO_2/Si$ substrates using ICP-CVD (inductively coupled plasma chemical vapor deposition). A 10 nm-Ni layer was then deposited by e-beam evaporation. Finally, 10 nm-Ni/60 nm a-Si:H/200 nm-$SiO_2/Si$ and 10 nm-Ni/20 nm a-Si:H/200 nm-$SiO_2/Si$ structures were prepared. The samples were annealed by rapid thermal annealing for 40 seconds at $200{\sim}500^{\circ}C$ to produce $NiSi_x$. The resulting changes in sheet resistance, microstructure, phase, chemical composition and surface roughness were examined. The nickel silicide on a 60 nm a-Si:H substrate showed a low sheet resistance at T (temperatures) >$450^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate showed a low sheet resistance at T > $300^{\circ}C$. HRXRD analysis revealed a phase transformation of the nickel silicide on a 60 nm a-Si:H substrate (${\delta}-Ni_2Si{\rightarrow}{\zeta}-Ni_2Si{\rightarrow}(NiSi+{\zeta}-Ni_2Si)$) at annealing temperatures of $300^{\circ}C{\rightarrow}400^{\circ}C{\rightarrow}500^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate had a composition of ${\delta}-Ni_2Si$ with no secondary phases. Through FE-SEM and TEM analysis, the nickel silicide layer on the 60 nm a-Si:H substrate showed a 60 nm-thick silicide layer with a columnar shape, which contained both residual a-Si:H and $Ni_2Si$ layers, regardless of annealing temperatures. The nickel silicide on the 20 nm a-Si:H substrate had a uniform thickness of 40 nm with a columnar shape and no residual silicon. SPM analysis shows that the surface roughness was < 1.8 nm regardless of the a-Si:H-thickness. It was confirmed that the low temperature silicide process using a 20 nm a-Si:H substrate is more suitable for thin film transistor (TFT) active layer applications.