• Title/Summary/Keyword: Fe-SEM

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Surface Morphology of PEO-treated Ti-6Al-4V Alloy after Anodic Titanium Oxide Treatment (ATO 처리후, 플라즈마 전해 산화 처리된 Ti-6Al-4V 합금의 표면 형태)

  • Kim, Seung-Pyo;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.75-75
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    • 2018
  • Commercially pure titanium (CP-Ti) and Ti-6Al-4V alloys have been widely used in implant materials such as dental and orthopedic implants due to their corrosion resistance, biocompatibility, and good mechanical properties. However, surface modification of titanium and titanium alloys is necessary to improve osseointegration between implant surface and bone. Especially, when titanium oxide nanotubes are formed on the surface of titanium alloy, cell adhesion is greatly improved. In addition, plasma electrolytic oxide (PEO) coatings have a good safety for osseointegration and can easily and quickly form coatings of uniform thickness with various pore sizes. Recently, the effects of bone element such as magnesium, zinc, strontium, silicon, and manganese for bone regeneration are researching in dental implant field. The purpose of this study was researched on the surface morphology of PEO-treated Ti-6Al-4V alloy after anodic titanium oxide treatmentusing various instruments. Ti-6Al-4V ELI disks were used as specimens for nanotube formation and PEO-treatment. The solution for the nanotube formation experiment was 1 M $H_3PO_4$ + 0.8 wt. % NaF electrolyte was used. The applied potential was 30V for 1 hours. The PEO treatment was performed after removing the nanotubes by ultrasonics for 10 minutes. The PEO treatment after removal of the nanotubes was carried out in the $Ca(CH_3)_2{\cdot}H_2O+(CH_3COO)_2Mg{\cdot}4H_2O+Mn(CH_3COO)_2{\cdot}4H_2O+Zn(CH_3CO_2)_2Zn{\cdot}2H_2O+Sr(CH_2COO)_2{\cdot}0.5H_2O+C_3H_7CaO_6P$ and $Na_2SiO_3{\cdot}9H_2O$ electrolytes. And the PEO-treatment time and potential were 3 minutes at 280V. The morphology changes of the coatings on Ti-6Al-4V alloy surface were observed using FE-SEM, EDS, XRD, AFM, and scratch tester. The morphology of PEO-treated surface in 5 ion coating solution after nanotube removal showed formation or nano-sized mesh and micro-sized pores.

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A Study on the Self-cleaning Surface Finishing Using PFOA Free Fluoric Polymer and Silica Nano-sol (PFOA Free 불소 고분자 및 실리카 나노졸을 이용한 self cleaning 표면 가공에 관한 연구)

  • Park, Sung-Min;Kwon, Il-Jun;Kim, Ran;Yeum, Jeong-Hyun;Yoon, Nam-Sik;Lee, Kyeung-Nam
    • Textile Coloration and Finishing
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    • v.21 no.6
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    • pp.1-11
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    • 2009
  • Super-hydrophobic surface, with a water contact angle greater than $150^{\circ}$, has a self cleaning effect termed 'lotus effect'. We introduced super-hydrophobicity onto aramid/rayon mixture fabric with dual-scale structure by assembling silica nano-sol. Mixture fabric was treated with silica nano-sol, fluoric polymer using various parameters such as particle size, concentration. Silica nano-sol size were measured using particle size analyzer. Morphological changes by particle size were observed using field emission scanning electron microscopy(FE-SEM), contact angle measurement equipment. The contact angle of water was about $134.0^{\circ}$, $137.0^{\circ}$, $143.0^{\circ}$, $139.5^{\circ}$ and $139.0^{\circ}$ for mixture fabric coated with 100.2nm, 313.7nm, 558.2nm, 628.5nm and 965.4nm silica nano-sol, compared with about $120.0^{\circ}$ for mixture fabric coated with fluoric polymer. When we mixed particle sizes of 100.2nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $146.2^{\circ}$. And we mixed particle sizes of 313.7nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $141.8^{\circ}$. Also we mixed particle sizes of 558.2nm and 965.4nm by 7:3 volume ratio, the best super-hydrophobicity was obtained. In this paper, we fabricated the water-repellent surfaces with various surface structures by using four types of silica nano-sol, and we found that the dual-scale structure was very important for the super-hydrophobicity.

Cu Electroplating on the Si Wafer and Reliability Assessment of Low Alpha Solder Bump for 3-D Packaging (3차원 실장용 실리콘 웨이퍼 Cu 전해도금 및 로우알파솔더 범프의 신뢰성 평가)

  • Jung, Do Hyun;Lee, Joon Hyung;Jung, Jae Pil
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2012.11a
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    • pp.123-123
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    • 2012
  • 최근 연구되고 있는 TSV(Through Silicon Via) 기술은 Si 웨이퍼 상에 직접 전기적 연결 통로인 관통홀을 형성하는 방법으로 칩간 연결거리를 최소화 할 수 있으며, 부피의 감소, 연결부 단축에 따른 빠른 신호 전달을 가능하게 한다. 이러한 TSV 기술은 최근의 초경량화와 고집적화로 대표되는 전자제품의 요구를 만족시킬 수 있는 차세대 실장법으로 기대를 모으고 있다. 한편, 납땜 재료의 주 원료인 주석은 주로 반도체 소자의 제조, 반도체 칩과 기판의 접합 및 플립 칩 (Flip Chip) 제조시의 범프 형성 등 반도체용 배선재료에 널리 사용되고 있다. 최근에는 납의 유해성 때문에 대부분의 전자제품은 무연솔더를 이용하여 제조되고 있지만, 주석을 이용한 반도체 소자가 고밀도화, 고 용량화 및 미세피치(Fine Pitch)화 되고 있기 때문에, 반도체 칩의 근방에 배치된 주석으로부터 많은 알파 방사선이 방출되어 메모리 셀의 정보를 유실시키는 소프트 에러 (Soft Error)가 발생되는 위험이 많아지고 있다. 이로 인해, 반도체 소자 및 납땜 재료의 주 원료인 주석의 고순도화가 요구되고 있으며, 특히 알파 방사선의 방출이 낮은 로우알파솔더 (Low Alpha Solder)가 요구되고 있다. 이에 따라 본 연구는 4인치 실리콘 웨이퍼상에 직경 $60{\mu}m$, 깊이 $120{\mu}m$의 비아홀을 형성하고, 비아 홀 내에 기능 박막증착 및 전해도금을 이용하여 전도성 물질인 Cu를 충전한 후 직경 $80{\mu}m$의 로우알파 Sn-1.0Ag-0.5Cu 솔더를 접합 한 후, 접합부 신뢰성 평가를 수행을 위해 고속 전단시험을 실시하였다. 비아 홀 내 미세구조와 범프의 형상 및 전단시험 후 파괴모드의 분석은 FE-SEM (Field Emission Scanning Electron Microscope)을 이용하여 관찰하였다. 연구 결과 비아의 입구 막힘이나 보이드(Void)와 같은 결함 없이 Cu를 충전하였으며, 고속전단의 경우는 전단 속도가 증가할수록 취성파괴가 증가하는 경향을 보였다. 본 연구를 통하여 전해도금을 이용한 비아 홀 내 Cu의 고속 충전 및 로우알파 솔더 볼의 범프 형성이 가능하였으며, 이로 인한 전자제품의 소프트에러의 감소가 기대된다.

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PHOTOCATALYTIC ANTIEUNGAL ACTIVITY AGAINST CANDIDA ALBICANS BY $TiO_2$ COATED ACRYLIC RESIN DENTURE BASE

  • Yang Ji-Yeon;Kim Hee-Jung;Chung Chae-Heon
    • The Journal of Korean Academy of Prosthodontics
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    • v.44 no.3
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    • pp.284-294
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    • 2006
  • Statement of problem. Proliferation of Candida albicans is primarily within the plaque on the fitting surface of the denture rather than on the inflamed mucosa. Consequently, the treatment of the denture is equally important as treatment of the tissue. Cleansing and disinfection should be efficiently carried-out as the organisms can penetrate into the voids of the acrylic resin and grow in them, from which they can continue to infect and reinfect bearing tissues. Purpose. The purpose of this study was to evaluate the applicability of photocatalytic reaction to eliminate Candida albicans from acrylic resin denture base, and to investigate the anti-fungal effect with various UVA illumination time. Materials and Methods. The specimens were cured by the conventional method following the manufacturer's instruction using thermal polymerized denture base resin (Vertex RS: Dentimex, Netherlands). $TiO_2$ photocatalyst sol(LT), which is able to be coated at normal temperature, was made from the Ti-alkoxide progenitor. The XRD patterns, TEM images and nitrogen absorption ability of the $TiO_2$ photocatalyst sol(LT) were compared with the commercial $TiO_2$ photocatalyst P-25. The experimental specimens were coated with the mixture of the $TiO_2$ photocatalyst sol(LT) and binder material (silane) using dip-coater, and uncoated resin plates were used as the control group. Crystallinity of $TiO_2$ of the specimen was tested by the XRD. Size, shape and chemical compositions were also analyzed using the FE-SEM/ EDS. The angle and methylene blue degradation efsciency were measured for evaluating the photocatalytic activity of the $TiO_2$ film. Finally, the antifungal activity of the specimen was tested. Candida albicans KCTC 7629(1 ml, initial concentration $10^5$ cells/ ml) were applied to the experiment and control group specimens and subsequently two UVA light source with 10W, 353 nm peak emission were illuminated to the specimens from 15cm above. The extracted $2{\mu}l$ of sample was plated on nutrient agar plate ($Bacto^{TM}$ Brain Heart Infusion; BD, USA) with 10 minute intervals for 120 minute, respectively. It was incubated for 24 hours at $37^{\circ}C$ and the colony forming units (CFUs) were then counted. Results. Compared the characteristics of LT photocatalyst with commercial P-25 photocatalyst, LT were shown higher activity than P-25. The LT coated experimental specimen surface had anatase crystal form, less than 20 nm of particle size and wide specific surface area. To evaluate the photocatalytic activity of specimens, methylene blue degradation reaction were used and about 5% of degradation rate were measured after 2 hours. The average contact angle was less than $20^{\circ}$ indicating that the LT photocatalyst had hydrophilicity. In the antifungal activity test for Candida albicans, 0% survival rate were measured within 30 minute after irradiation of UVA light. Conclusion. From the results reported above, it is concluded that the UVA-LT photocatalytic reaction have an antifungal effect on the denture surface Candida albicans, and so that could be applicable to the clinical use as a cleaning method.

MECHANICAL PROPERTIES OF TIN COATED FILM WITH VARIOUS COATING THICKNESS ON TITANIUM ALLOY (타이타늄 합금에 다양한 두께로 코팅된 TiN 피막의 기계적 성질)

  • Lee, Jae-Yun;Oh, Dong-Joon;Kim, Hee-Jung;Chung, Chae-Heon
    • The Journal of Korean Academy of Prosthodontics
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    • v.45 no.5
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    • pp.675-686
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    • 2007
  • Statement of problem: Titanium nitride(TiN) coatings are the most general and popular coating method and used to improve the properties of metallic surface for industrial purposes. When TiN coating applied to the abutment screw, frictional resistance would be reduced, as a results, the greater preload and prevention of the screw loosening could be expected. Purpose: The purpose of this study was to investigate mechanical properties of TiN coated film of various coating thickness on the titanium alloy surface and to evaluate proper coating thickness. Material and method: 95 Titanium alloy (Ti-6Al-4V) discs of 15 mm in diameter and 3 mm in thickness were prepared for TiN coating and divided into 7 groups in this study. Acceding to coating deposition time (CDT) with TiN by using Arc ion plating, were divided into 7 groups : Group A (CDT 30min), Group B (CDT 60min), Group C (CDT 90min), Group D (CDT 120min), Group E (CDT 150min), Group F(CDT 180min) and Group G (no CDT) as a control group. TiN coating surface was observed with Atomic Force Microscope(AFM), field emission scanning electron microscopy(FE-SEM) and examined with scratch tester, wear tester. Result: 1. Coating thickness fir each coated group was increased in proportion to coating deposition time. 2. Surface of all coated groups except Group A was homogeneous and smooth. However, surface of none coated Group G had scratch. 3. Adhesion strength for each coated group was increased in proportion to coating deposition time. 4. Wear resistance for each coated group was increased in proportion to coating deposition time. 5. Surface roughness in Group A, B, C was increased in proportion to coating deposition time. But, surface roughness in Group D, E, F was showed decreased tendency in proportion to coating deposition time. Conclusion: According to coating deposition time, mechanical properties of TiN coated film were changed. It was considered that 120 minutes coating deposition time ($1.32{\mu}m$ in coating thickness) is necessary.

Dye-Sensitized Solar Cell Based on TiO2-Graphene Composite Electrodes (TiO2와 Graphene 혼합물을 전극으로 사용한 염료감응형 태양전지특성 연구)

  • Battumur, T.;Yang, Wooseung;Ambade, S.B.;Lee, Soo-Hyoung
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.177-181
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    • 2012
  • Dye-sensitized solar cells(DSSCs) based on $TiO_2$ film photo anode incorporated with different amount of grapheme nanosheet(GNS) are fabricated and their photovoltaic performance are investigated. The $TiO_2$-GNS composite electrode has been prepared by a direct mixing method. The DSSC performance of this composite electrode was measured using N3 dye as a sensitizer. The performance of DSSCs using the $TiO_2$-GNS composite electrodes is dependent on the GNS loading in the electrodes. The results show that the DSSCs incorporating 0.01 wt% GNS in $TiO_2$photo anode demonstrates a maximum power conversion efficiency of 5.73%, 26% higher than that without GNS. The performance improvement is ascribed to increased N3 dye adsorption, the reduction of electron recombination and back transport reaction as well as enhancement of electron transport with the introduction of GNS. The presence of both $TiO_2$(anatase) and GNS has been confirmed by FieldEmission Scanning Electron Microscopy(FE-SEM). The decrease in recombination due to GNS in DSSCs has been investigated by the Electrochemical Impedance Spectroscopy.

Hydrothermal Synthesis and Mechanical Characterization of ZrO2 by Y2O3 Stabilizer Contents (Y2O3안정화제 첨가량에 따라 수열합성법으로 제조된 ZrO2-Xmol% Y2O3분말의 합성 및 기계적 특성)

  • Lee, Hak-Joo;Kim, Taik-Nam;Bea, Sung-Chul;Go, Myung-Won;Ryu, Jae-Kyung
    • Korean Journal of Materials Research
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    • v.20 no.10
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    • pp.518-523
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    • 2010
  • In this study, partially stabilized zirconia was synthesized using a chemical $Y_2O_3$ stabilizer and hydrothermal method. First, $YCl_3-6H_2O$ and $ZrCl_2O-8H_2O$ was dissolved in distilled water. Y-TZP (a $Y_2O_3$-doped toughened zirconia polycrystalline precursor) was also prepared by conventional co-precipitates in the presence of an excess amount of $NH_4OH$ solution under a fixed pH of 12. The Y-TZP precursors were filtered and repeatedly washed with distilled water to remove $Cl^-$ ions. $ZrO_2$-Xmol%$Y_2O_3$ powder was synthesized by a hydrothermal method using Teflon Vessels at $180^{\circ}C$ for 6 h of optimized condition. The powder added with the Xmol%- $Y_2O_3$ (X = 0,1,3,5 mol%) stabilizer of the $ZrO_2$ was synthesized. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens of $33mm{\times}8mm{\times}3$ mm for three-point bend tests were used in the mechanical properties evaluation. A teragonal phase was observed in the samples, which contains more than 3 mol% $Y_2O_3$. The $3Y-ZrO_2$ agglomerated particle size was measured at $7.01{\mu}m$. The agglomerated particle was clearly observed in the sample of 5 mol % $Y_2O_3-ZrO_2$, and and the agglomerated particle size was measured at 16.4 um. However, a 20 nm particle was specifically observed by FE-SEM in the sample of 3 mol% $Y_2O_3-ZrO_2$. The highest bending fracture strength was measured as 321.3 MPa in sample of 3 mol% $Y_2O_3-ZrO_2$.

Recycling Properties of Visible-Light Driven CdZnS/ZnO Photocatalyst Prepared by a Simple Precipitation Method (단순 침전법으로 제조한 가시광선용 CdZnS/ZnO 광촉매의 재활용 특성)

  • Lee, Gun Dae;Park, Seong Soo;Jin, Youngeup;Hong, Seong Soo
    • Clean Technology
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    • v.23 no.2
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    • pp.196-204
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    • 2017
  • CdZnS/ZnO composite was prepared through low-temperature precipitation and drying method. The property of CdZnS/ZnO as a recyclable photocatalyst for the degradation of rhodamine B (RhB) under visible light irradiation was examined. The sample was characterized by XRD, FE-SEM, XPS, UV-vis DRS and photoluminescence techniques before and after repeated reaction to investigate the change of properties during the photocatalytic reaction. During repeated reaction, the CdZnS/ZnO showed an improved photocatalytic activity and recycle stability. Among two feasible reaction pathways for photocatalytic degradation of RhB, the cleavage of conjugated chromophore was found to predominate over N-dealkylation of chromophore skeleton in the present work. The results indicate that the CdZnS/ZnO, prepared by a simple precipitation method, can be used as a visible-light driven photocatalyst with enhanced cycle stability and activity.

Corrosion Characteristics of TiN/Ti Multilayer Coated Ti-30Ta-xZr Alloy for Biomaterials (TiN/Ti 다층막 코팅된 생체용 Ti-30Ta-xZr 합금의 부식특성)

  • Kim, Y.U.;Cho, J.Y.;Choe, H.C.
    • Corrosion Science and Technology
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    • v.8 no.4
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    • pp.162-169
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    • 2009
  • Pure titanium and its alloys are drastically used in implant materials due to their excellent mechanical properties, high corrosion resistance and good biocompatibility. However, the widely used Ti-6Al-4V is found to release toxic ions (Al and V) into the body, leading to undesirable long-term effects. Ti-6Al-4V has much higher elastic modulus than cortical bone. Therefore, titanium alloys with low elastic modulus have been developed as biomaterials to minimize stress shielding. For this reason, Ti-30Ta-xZr alloy systems have been studied in this study. The Ti-30Ta containing Zr(5, 10 and 15 wt%) were 10 times melted to improve chemical homogeneity by using a vacuum furnace and then homogenized for 24 hrs at $1000^{\circ}C$. The specimens were cut and polished for corrosion test and Ti coating and then coated with TiN, respectively, by using DC magnetron sputtering method. The analyses of coated surface were carried out by field emission scanning electron microscope(FE-SEM). The electrochemical characteristics were examined using potentiodynamic (- 1500 mV~+ 2000 mV) and AC impedance spectroscopy(100 kHz~10 mHz) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. The equiaxed structure was changed to needle-like structure with increasing Zr content. The surface defects and structures were covered with TiN/Ti coated layer. From the polarization behavior in 0.9% NaCl solution, The corrosion current density of Ti-30Ta-xZr alloys decreased as Zr content increased, whereas, the corrosion potential of Ti-30Ta-xZr alloys increased as Zr content increased. The corrosion resistance of TiN/Ti-coated Ti-30Ta-xZr alloys were higher than that of the TiN-coated Ti-30Ta-xZr alloys. From the AC impedance in 0.9% NaCl solution, polarization resistance($R_p$) value of TiN/Ti coated Ti-30Ta-xZr alloys showed higher than that of TiN-coated Ti-30Ta-xZr alloys.

Influence of Copper Azole Retention Level to Wood Decay (목재 내 Copper Azole 보유량이 목재부후에 미치는 영향)

  • Lee, Hyun-Mi;Son, Dong-Won;Lee, Han-Sol;Hwang, Won-Joung
    • Journal of the Korean Wood Science and Technology
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    • v.43 no.1
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    • pp.112-121
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    • 2015
  • In this study, Copper Azole (CuAz), a domestically available wood preservative for pressure treatment, was employed to perform an experimental research on its infiltration and decay properties in Japanese Red Pine. Test specimens were pressure-injected with CuAz-2 preservative to measure its preservative effectiveness, and then its impact on weight and mass losses. Furthermore, wood specimens were treated with CuAz-2 preservatives of various concentration levels before they were decayed with brown-rot-fungi in order to observe decay properties on light microscope (LM) and field emission scanning electron microscope (FE-SEM). As a result, untreated specimen by Fomitopsis palustris showed the mass loss of more than 40%, and the value of preservative effectiveness of CuAz-2 by indoor decay was $1,73-3.32kg/m^3$. The concentration levels of CuAz-2 preservative were shown to cause significant variations in terms of decay progresses in the cross section, radial section, and tangential section. By contrast, untreated specimens had underwent serious decays in early wood, late wood, longitudinal resin canals, and ray, which led to vertical destruction of wood texture. As for the radial section, ray tracheid, ray parenchyma cell, and window like pits were decayed and destroyed. In the case of tangential section, uniseriate rays and vertical resin canals were seriously decayed. In conclusion, this study indicates that the adequacy of the current CuAz injection amount should be reviewed in the domestic environment because there are significantly different decays at different decay conditions.