• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.93-93
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• 2017

고전력 펄스 전원공급장치를 이용한 마그네트론 스퍼터링(high-power impulse magnetron sputtering; HiPIMS)과 직류(direct current; DC) 전원공급장치를 이용한 마그네트론 스퍼터링(DC 스퍼터링)을 이용하여 제조한 티타늄 질화물(titanium nitride; TiN) 박막의 특성을 비교하였다. HiPIMS와 DC 스퍼터링 공정 중에 빗각증착을 적용하여 TiN 박막의 미세구조와 기계적 특성의 변화를 확인하였다. TiN 박막을 코팅하기 위한 기판으로 스테인리스 강판(SUS304)과 초경(cemented carbide; WC-10wt.%Co)을 사용하였다. 기판은 알코올과 아세톤으로 초음파 처리를 실시하여 기판 표면의 불순물을 제거하였다. 기판 청정 후 진공용기 내부의 기판홀더에 기판을 장착하고 $2.0{\times}10^{-5}torr$의 기본 압력까지 진공배기를 실시하였다. 진공 용기의 압력이 기본 압력에 도달하면 아르곤(Ar) 가스를 진공용기 내부로 ${\sim}10^{-2}torr$의 압력으로 주입하고 기판홀더에 라디오 주파수(radio frequency; rf) 전원공급장치를 이용하여 - 800 V의 전압을 인가하여 글로우 방전을 발생시켜 30 분간 기판 표면의 산화막을 제거하는 기판청정을 실시하였다. 기판청정이 완료되면 기본 압력까지 진공배기를 실시하고 Ar과 질소($N_2$)의 혼합 가스를 진공용기 내부로 ${\sim}10^{-3}torr$의 압력으로 주입하여 HiPIMS와 DC 스퍼터링으로 TiN 박막 제조를 실시하였다. 빗각의 크기는 $45^{\circ}$와 $-45^{\circ}$이었다. 제조된 TiN 박막은 주사전자 현미경, 비커스 경도 측정기 그리고 X-선 회절 분석기를 이용하여 특성을 분석하였다. HiPIMS로 제조한 TiN 박막은 기판 전압을 인가하지 않아도 색상이 노란색을 보이지만, DC 스퍼터링으로 제조한 TiN 박막은 기판 전압을 인가하지 않으면 노란색을 보이지 않고 어두운 갈색에 가까운 색을 보였다. TiN 박막의 경도는 HiPIMS로 제조한 TiN 박막이 DC 스퍼터링으로 제조한 TiN 박막보다 높았다. 이러한 TiN 박막의 특성 차이는 DC 스퍼터링과 비교하여 높은 HiPIMS의 이온화율에 의한 결과로 판단된다. 빗각을 적용한 TiN 박막은 미세구조 변화를 보였으며 이러한 미세구조 변화는 TiN 박막의 특성에 영향을 미치는 것을 확인하였다.

• Korean Journal of Materials Research
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• v.23 no.7
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• pp.373-378
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• 2013

In order to clarify the effect of C/Ti atom ratios(${\chi}$) on the deformation behavior of $TiC_{\chi}$ at high temperature, single crystals having a wide range of ${\chi}$, from 0.56 to 0.96, were deformed by compression test in a temperature range of 1183~2273 K and in a strain rate range of $1.9{\times}10^{-4}{\sim}5.9{\times}10^{-3}s^{-1}$. Before testing, $TiC_{\chi}$ single crystals were grown by the FZ method in a He atmosphere of 0.3MPa. The concentrations of combined carbon were determined by chemical analysis and the lattice parameters by the X-ray powder diffraction technique. It was found that the high temperature deformation behavior observed is the ${\chi}$-less dependent type, including the work softening phenomenon, the critical resolved shear stress, the transition temperature where the deformation mechanism changes, the stress exponent of strain rate and activation energy for deformation. The shape of stress-strain curves of $TiC_{0.96}$, $TiC_{0.85}$ and $TiC_{0.56}$ is seen to be less dependent on ${\chi}$, the work hardening rate after the softening is slightly higher in $TiC_{0.96}$ than in $TiC_{0.85}$ and $TiC_{0.56}$. As ${\chi}$ decreases the work softening becomes less evident and the transition temperature where the work softening disappears, shifts to a lower temperature. The ${\tau}_c$ decreases monotonously with decreasing ${\chi}$ in a range of ${\chi}$ from 0.86 to 0.96. The transition temperature where the deformation mechanism changes shifts to a lower temperature as ${\chi}$ decreases. The activation energy for deformation in the low temperature region also decreased monotonously as ${\chi}$ decreased. The deformation in this temperature region is thought to be governed by the Peierls mechanism.

• Journal of the Korean institute of surface engineering
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• v.46 no.5
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• pp.216-222
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• 2013

In order to improve the performance of electrodeposited diamond-nickel composite, surface modification of diamond particles was carried out using powder immersion reaction assisted coating (PIRAC). Titanium and chromium were selected as coating elements, which are known as carbide former. With respect to the powder elements, various phases were formed on diamond; metallic Ti and TiC for Ti powder, $Cr_3C_2$ for Cr powder, and TiC and $Cr_3C_2$ for Ti-Cr mixed powder. Surface modified diamond particle showed higher specific surface area, especially Ti coating induced considerable increase of specific surface area. The increase of specific surface area suggests increase of surface roughness, and that was confirmed by surface observation using FE-SEM. In addition, wear properties of diamond-nickel composite including surface modified diamonds were improved, and Ti coated diamond showed the highest performance. The wear property of diamond-nickel composite is dependent on adhesion strength between diamond particle and nickel layer. Therefore, surface modification of diamond particle by PIRAC increasing surface roughness is effective to improve the properties of diamond-nickel composite.

• The Journal of Korean Academy of Prosthodontics
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• v.46 no.5
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• pp.500-510
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• 2008

Statement of problem: Recently researches about WC/C (Tungsten Carbide/Carbon) or TiN (Titanium Nitride) coating on abutment screws are going on. It decreases friction coefficient, resistance against corrosion and withdrawal of physical fragility when the coating is applied to the metal surfaces. It is reported that coated abutment screws improved abrasion, adaptability and detorque force. Purpose: This study is about the effects of coated abutment screws on loosening of screw and for the purpose of solving the loosening phenomenon of abutment screws which is clinical problem. Material and methods: Detorque force and surface changes are compared when 10 times of repeated closing and opening are applied to both uncoated titanium abutment screws (Group A) and coated abutment screws with WC/C (Group B) and TiN (Group C). Each group was made up of 10 abutment screws. Results: 1. Before repeated closing and opening, Somewhat rough surface with regular direction was observed in Group A. Coated granules were observed in group B and group C and overall coated layer appeared in regular and smooth form. 2. Before repeated closing and opening, The coated surface showed bigger and thicker size of coated granules in Group C than Group B. 3. After repeated closing and opening, abrasion and deformation of abutment screw surface was observed in Group A and Group B. Exfoliation phenomenon was observed in Group B. 4. Group A showed biggest range of decrease when the weight changes of abutment screws were measured before and after repeated closing and opening. Group C showed less weight changes than Group B but there was no statistical difference between two groups. 5. Group B and Group C showed higher average detorque force than Group A and there was statistical difference. 6. Group A showed more prominent decrease tendency of average detorque force than Group B and Group C. Conclusion: Coated abutment screws with WC/C or TiN did not show prominent surface changes than uncoated titanium abutment screws even though they were repeatedly used. And they showed excellent resistance against friction and high detorque force. Thus it is considered that adaptation of WC/C or TiN coating on abutment screws will improve the screw loosening problem.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.251-251
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• 2016

For several decades, industrial processes consume a huge amount of raw water for various objects that consequently results in the generation of large amounts of wastewater. Wastewaters are consisting of complex mixture of different inorganic and organic compounds and some of them can be toxic, hazardous and hard to degrade. These effluents are mainly treated by conventional technologies such are aerobic and anaerobic treatment and chemical coagulation. But, these processes are not suitable for eliminating all hazardous chemical compounds form wastewater and generate a large amount of toxic sludge. Therefore, other processes have been studied and applied together with these techniques to enhance purification results. These include photocatalysis, absorption, advanced oxidation processes, and ozonation, but also have their own drawbacks. In recent years, electrochemical techniques have received attention as wastewater treatment process that could be show higher purification results. Among them, boron doped diamond (BDD) attract attention as electrochemical electrode due to good chemical and electrochemical stability, long lifetime and wide potential window that necessary properties for anode electrode. So, there are many researches about high quality BDD on Nb, Ta, W and Si substrates, but, their application in effluents treatment is not suitable due to high cost of metal and low conductivity of Si. To solve these problems, Ti has been candidate as substrate in consideration of cost and property. But there are adhesion issues that must be overcome to apply Ti as BDD substrate. Al, Cu, Ti and Nb thin films were deposited on Ti substrate to improve adhesion between substrate and BDD thin film. In this paper, BDD films were deposited by hot filament chemical vapor deposition (HF-CVD) method. Prior to deposition, cleaning processes were conducted in acetone, ethanol, and isopropyl alcohol (IPA) using sonification machine for 7 min, respectively. And metal layer with the thickness of 200 nm were deposited by DC magnetron sputtering (DCMS). To analyze microstructure X-ray diffraction (XRD, Bruker gads) and field emission scanning electron microscopy (FE-SEM, Hitachi) were used. It is confirmed that metal layer was effective to adhesion property and improved electrode property. Electrochemical measurements were carried out in a three electrode electrochemical cell containing a 0.5 % H2SO4 in deionized water. As a result, it is confirmed that metal inter layer heavily effect on BDD property by improving adhesion property due to suppressing formation of titanium carbide.

• Proceedings of the KWS Conference
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• 2002.10a
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• pp.250-254
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• 2002

Intergranular corrosion of austenitic stainless steels is a conventional and momentous problem during welding and high temperature use. One of the major reasons for such intergranular corrosion is so-called sensitization, i.e., chromium depletion due to chromium carbide precipitation at grain boundaries. Conventional methods for preventing sensitization of austenitic stainless steels include reduction of carbon content in the material, stabilization of carbon atoms as non-chromium carbides by the addition of titanium, niobium or zirconium, local solution-heat-treatment by laser beam, etc. These methods, however, are not without drawbacks. Recent grain boundary structure studies have demonstrated that grain boundary phenomena strongly depend on the crystallographic nature and atomic structure of the grain boundary, and that grain boundaries with coincidence site lattices are immune to intergranular corrosion. The concept of "grain boundary design and control", which involves a desirable grain boundary character distribution, has been developed as grain boundary engineering. The feasibility of grain boundary engineering has been demonstrated mainly by thermomechanical treatments. In the present study, a thermomechanical treatment was tried to improve the resistance to the sensitization by grain boundary engineering. A type 304 austenitic stainless steel was pre-strained and heat-treated, and then sensitized, varying the parameters (pre-strain, temperature, time, etc.) during the thermomechanical treatment. The grain boundary character distribution was examined by orientation imaging microscopy. The intergranular corrosion resistance was evaluated by electrochemical potentiokinetic reactivation and ferric sulfate-sulfuric acid tests. The sensitivity to intergranular corrosion was reduced by the thermomechanical treatment and indicated a minimum at a small roll-reduction. The frequency of coincidence-site-lattice boundaries indicated a maximum at a small strain. The ferric sulfate-sulfuric acid test showed much smaller corrosion rate in the thermomechanically-treated specimen than in the base material. An excellent intergranular corrosion resistance was obtained by a small strain annealing at a relatively low temperature for long time. The optimum parameters created a uniform distribution of a high frequency of coincidence site lattice boundaries in the specimen where corrosive random boundaries were isolated. The results suggest that the thermomechanical treatment can introduce low energy segments in the grain boundary network by annealing twins and can arrest the percolation of intergranular corrosion from the surface.

• Korean Journal of Materials Research
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• v.14 no.12
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• pp.893-899
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• 2004

Even though Ti-6Al-4V has gained popularity as an implant material, the possible dissolution of Al and V ions in body fluids remains a matter of concern. Though commercially pure Ti (Cp-Ti) overcomes this problem, the mechanical strength of pure titanium remains very low. Thus, in this experiment Cp-Ti was processed by Equal channel angular processing (ECAP), in order to increase the mechanical strength. The biocompatibility of ECAP-Ti, Cp-Ti and Ti-6Al-4V was examined by the apatite formation on each sample surface, after treating the surface with 5M NaOH and soaking in Simulated body fluids (SBF). Initially, the samples were mechanically polished on silicone carbide paper (#2000). The polished samples were treated with 5M NaOH solution at $60^{\circ}C$ for 24 hours. The NaOH treated samples were washed gently with distill water and dried at $40^{\circ}C$ for 1 day. The dried samples were heat treated in air at $600^{\circ}C$ for 1 hour. The surface morphology of these samples were studied using SEM and XRD. The SEM studies showed network of pores in all samples. The XRD showed oxide layer formation on Cp-Ti and Ti-6Al-4V. samples. However the oxide layer in ECAP-Ti was not substantial. These samples were immersed in SBF, kept at $36.5^{\circ}C$ for seven days period. At the end of 7 days, the apatite formation was confirmed only on Cp-Ti and was not observed in Ti-6Al-4V and ECAP-Ti. These observations of apatite formation relate to the fact that Cp-Ti showed greater oxide layer than other samples. The apatite examined was confirmed as tricalcium phosphate (TCP) using EDS and XRD.

• The Journal of Engineering Research
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• v.6 no.2
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• pp.23-32
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• 2004

Metals, ceramics and polymers are widely used as bioimplant materials. However, Ti and Ti alloys are widely used because of its high strength to weight ratio and good biocompatibility when implanted in the body. In this experiment, Ti alloys of Grade-4 (gr4), 0.2 wt % Fe, 0.5 wt % Fe and 2 wt % Fe were studied for their surface morphology and HAp forming ability on the metal substrate for different treatments. Intially, the samples were mechanically polished on silicone carbide paper (No.-2000). The polished samples were treated with 5M NaOH solution at $60^{\circ}C$ for 24 hours. The NaOH treated samples were washed gently with distill water and dried at $40^{\circ}C$ for 1 day. The dried samples were heated in air at $600^{\circ}C$ for 1 hour. The surface morphology of these samples were studied using SEM. The SEM studies showed network of pores in all samples. These samples were immersed in stimulated body fluids (SBF) kept at $36.5^{\circ}C$ for different periods over the length of 1 to 14 days. The apatite formation was confirmed on all Ti-alloys using EDAX.

• Journal of Dental Rehabilitation and Applied Science
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• v.30 no.3
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• pp.206-214
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• 2014

This study is to evaluate how different bearing surface angles of abutment screw affect the mechanical stability of the joint in the conical seal design implant system. Materials and Methods: Internal connection type regular implants, two-piece cemented type abutments and tungsten carbide/carbon-coated titanium alloy abutment screws were selected. Titanium alloy screws with conical ($45^{\circ}$) and flat ($90^{\circ}$) head designs which fit on to abutment were fabricated. The abutments were tightened to implants with 30 Ncm by digital torque gauge. The loading was applied once to the central axis of abutment. The mean axial displacement was measured using micrometer before and after the tightening and loading (n = 5). The abutment was tightened to implants with 30 Ncm and T-shape stainless steel crown was cemented. Then the change in the amount of reverse-torque was measured after the repeated loading to the central axis, and the place 5 mm away from the central axis. Compressive bending and fatigue strength were measured at the place 5 mm away from the central axis (n = 5). Results: Both groups showed the largest axial displacement when abutment screw tightening and total displacement was greater in the flat head group compared to conical head group (P < 0.05). However, there were no significant differences in reverse torque value, compressive bending and fatigue strength (P > 0.05). Conclusion: Within the limitations of this study, the abutment screw head design had no effect on two groups regarding the joint stability, however the conical head design affected the settlement of abutment resulting in the reduced total displacement.