• Title/Summary/Keyword: FE-SEM/EDS

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Electrochemical Characteristics of Zn and Si Ion-doped HA Films on Ti-6Al-4V by PEO Treatment

  • Lim, Sang-Gyu;Hwang, In-Jo;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.199-199
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    • 2016
  • Commercially pure titanium (cp-Ti) and Ti alloys (typically Ti-6Al-4V) display excellent corrosion resistance and biocompatibility. Although the chemical composition and topography are considered important, the mechanical properties of the material and the loading conditions in the host have, conventionally. Ti and its alloys are not bioactive. Therefore, they do not chemically bond to the bone, whereas they physically bond with bone tissue. The electrochemical deposition process provides an effective surface for biocompatibility because large surface area can be served to cell proliferation. Electrochemical deposition method is an attractive technique for the deposition of hydroxyapatite (HAp). However, the adhesions of these coatings to the Ti surface needs to be improved for clinical used. Plasma electrolyte oxidation (PEO) enables control in the chemical com position, porous structure, and thickness of the $TiO_2$ layer on Ti surface. In addition, previous studies h ave concluded that the presence of $Ca^{+2}$ and ${PO_4}^{3-}$ ion coating on porous $TiO_2$ surface induced adhesion strength between HAp and Ti surface during electrochemical deposition. Silicon (Si) in particular has been found to be essential for normal bone and cartilage growth and development. Zinc (Zn) plays very important roles in bone formation and immune system regulation, and is also the most abundant trace element in bone. The objective of this work was to study electrochemical characteristcs of Zn and Si coating on Ti-6Al-4V by PEO treatment. The coating process involves two steps: 1) formation of porous $TiO_2$ on Ti-6Al-4V at high potential. A pulsed DC power supply was employed. 2) Electrochemical tests were carried out using potentiodynamic and AC impedance methoeds. The morphology, the chemical composition, and the micro-structure an alysis of the sample were examined using FE-SEM, EDS, and XRD. The enhancements of the HAp forming ability arise from $Si/Zn-TiO_2$ surface, which has formed the reduction of the Si/Zn ions. The promising results successfully demonstrate the immense potential of $Si/Zn-TiO_2$ coatings in dental and biomaterials applications.

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Millimeter-Scale Aligned Carbon Nanotubes Synthesized by Oxygen-Assisted Microwave Plasma CVD (MPCVD를 이용하여 밀리미터 길이로 수직 정렬된 탄소나노튜브의 합성)

  • Kim, Y.S.;Song, W.S.;Lee, S.Y.;Choi, W.C.;Park, C.Y.
    • Journal of the Korean Vacuum Society
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    • v.18 no.3
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    • pp.229-235
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    • 2009
  • Millimeter-scale aligned arrays of thin-multiwalled carbon nanotube (t-MWCNT) on layered Si substrates have been synthesized by oxygen-assisted microwave plasma chemical vapor deposition (MPCVD). We have succeeded in growth of vertically aligned MWCNTs up to 2.7 mm in height for 150 min. The effect of $O_2$ and water vapour on growth rate was systematically investigated. In the case of $O_2$ gas, the growth rate was ${\sim}22{\mu}m/min$, which is outstanding growth rate comparing with those of conventional thermal CVD (TCVD). Scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), and Raman spectroscopy were used to analyze the CNT morphology, composition and growth mechanism. The role of $O_2$ gas during the CNT growth was discussed on.

Antibacterial Effect of Gelatin/Ag Nanoparticle Biocomposite Prepared Using Solution Plasma Generated by Unipolar DC Power (단극성 직류전원으로 유도된 용액 플라즈마를 이용하여 제조한 젤라틴/은 나노입자 생체복합재료의 항균 효과)

  • Kim, Seong-Cheol;Yoon, Gook-Jin;Nam, Sang-Woo;Lee, Sang-Yul;Kim, Jung-Wan
    • Microbiology and Biotechnology Letters
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    • v.40 no.4
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    • pp.403-408
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    • 2012
  • Gelatin/Ag nanoparticle (AgNP) biocomposite was synthesized using the solution plasma process (SPP) that has been recently introduced as an effective method for synthesis of nanoparticles. In this study, gelatin/AgNP biocomposite was synthesized using various concentrations of Ag precursor ($AgNO_3$) and gelatin in the range of 1-5 mM and 1-3% (w/w), respectively, without using any chemical reducing agent. Physical properties of the gelatin/AgNP biocomposites were analyzed using EDS, FE-SEM, and TEM. The results indicated that spherical AgNPs with approximately 12~20 nm in diameter were synthesized successfully in the gelatin matrix by SPP. As the concentration of gelatin was increased (3%, w/w), disperse stability of AgNP was improved and micro-pores of gelatin became smaller and denser in the 3D scaffold. Bactericidal activity of the AgNPs was examined against Staphylococcus aureus and Escherichia coli by measuring zone of growth inhibition and decrease in colony forming unit (CFU). CFUs of S. aureus and E. coli were decreased approximately to 56% and 0%, respectively, by the gelatin/AgNP biocomposite, Ag5G3.

Microstructure of Co-base superalloy prepared by a investment casting (정밀주조법으로 제조된 Co계 초내열 합금의 미세구조)

  • Lee, Jung-Il;Lee, Ho Jun;Cho, Hyun Su;Paeng, Jong Min;Park, Jong Bum;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.6
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    • pp.313-318
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    • 2017
  • The microstructure of a cobalt-base superalloy (ECY768) obtained by an investment casting process was studied. This work focuses on the resulting microstructures arising from different melt and mold temperatures in normal industrial environmental conditions. The characterization of the samples was carried out using optical microscopy, field emission scanning electron microscopy and energy-dispersive spectroscopy. In this study, the as-cast microstructure is an ${\alpha}-Co$ (face-centered cubic) dendritic matrix with the presence of a secondary phase, such as $M_{23}C_6-type$ carbides precipitated at grain boundaries. These precipitates are the main strengthening mechanism in this type of alloy. Other minority phases, such as the MC-type phase, was also detected and their presence could be linked to the manufacturing process and environment.

Stability of TiN and WC Coated Dental Abutment Screw (TiN 및 WC코팅된 치과용 어버트먼트 나사의 안정성)

  • Son, M.K.;Lee, C.H.;Chung, C.H.;Jeong, Y.H.;Choe, H.C.
    • Journal of the Korean institute of surface engineering
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    • v.41 no.6
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    • pp.292-300
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    • 2008
  • Dental implant system is composed of abutment, abutment screw and implant fixture connected with screw. The problems of loosening/tightening and stability of abutment screw depend on surface characteristics, like a surface roughness, coating materials and friction resistance and so on. For this reason, surface treatment of abutment screw has been remained research problem in prosthodontics. The purpose of this study was to investigate the stability of TiN and WC coated dental abutment screw, abutment screw was used, respectively, for experiment. For improving the surface characteristics, TiN and WC film coating was carried out on the abutment screw using EB-PVD and sputtering, respectively. In order to observe the coating surface of abutment screw, surfaces of specimens were characterized, using field emission scanning electron microscope(FE-SEM) and energy dispersive x-ray spectroscopy(EDS). The stability of TiN and WC coated abutment screw was evaluated by potentiodynamic, and cyclic potentiodynamic polarization method in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. The corrosion potential of TiN coated specimen was higher than those of WC coated and non-coated abutment screw. Whereas, corrosion current density of TiN coated screws was lower than those of WC coated and non-coated abutment screw. The stability of screw decreased as following order; TiN coating, WC coating and non-coated screw. The pitting potentials of TiN and WC coated specimens were higher than that of non-coated abutment screw, but repassivation potential of WC coated specimen was lower than those of TiN coated and non-coated abutment screws due to breakdown of coated film. The degree of local ion dissolution on the surface increased in the order of TiN coated, non-coated and WC coated screws.

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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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.

A Scientific Analysis of Decorative Metal Foil Used in Pouch for the Sutra Embroidered with a Sun and Moon Design Designated as National Folklore Cultural Heritage (국가민속문화재 일월수 다라니 주머니 금속 장식지의 과학적 분석)

  • Pak, Seonghee;Park, Serin;Seo, Jeong Hun;Park, Jongseo;Lee, Ryangmi
    • Journal of Conservation Science
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    • v.38 no.2
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    • pp.124-132
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    • 2022
  • Through scientific analysis, this study identified the material characteristics of metal foil decorating the border line and knotting of the National Folklore Cultural Heritage 'Pouch for the Sutra Embroidered with a Sun and Moon Design'. Through Scanning Electron Microscope-Energy Dispersive Spectroscopy results, it was estimated that silver (Ag) and sulfur (S) were present in the metal foil, and silver leaf was also attached to the medium. S may discolor Ag from yellow to black depending on its concsentration and contact time. Yellow color could not be identified in metal foil at present. But there existed an example of the preparation of a gold-colored flat silver thread; therefore, further research is needed to estimate the original color. The lamella was reddish brown on the back. Aluminum, silicon, and iron were also detected and were the main components found in red soil. This is believed to be the red adhesive in traditional flat gold thread and is considered to be an adhesive-related component of the metal foil. From the gas chromatography mass spectrometry results, the adhesive component was confirmed to be animal glue.

Analysis of High-Temperature Corrosion of Heat Exchanger Tubes in Biomass Circulating Fluidized Bed Boiler (바이오매스 순환유동층 보일러의 열교환기 고온 부식 특성)

  • Yujin Choi;Dal-hee Bae;Doyeon Lee
    • Korean Chemical Engineering Research
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    • v.61 no.3
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    • pp.419-425
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    • 2023
  • This paper presents the research results of analyzing the high-temperature corrosion characteristics of three currently commercialized heat exchanger tube materials under actual operating conditions of a biomass power plant. In order to precisely analyze the high-temperature corrosion characteristics of these materials, a high-temperature corrosion evaluation device was installed in the power plant equipment, which allows for adjusting the surface temperature of the heat exchanger tubes. Experiments were conducted for approximately 300 hours under various temperature and operating conditions. In this study, the commercialized heat exchanger tube materials used were SA213T12, SA213T22, and SA213T91 alloys. In order to objectively analyze the high-temperature corrosion characteristics of each material, an international standard-based process to remove corrosion products was applied to obtain the weight change of the specimens, and the average thickness loss and corrosion rate were derived. Thus, the high-temperature corrosion results for each condition were quantitatively compared and analyzed. In addition, in order to increase the reliability of the high-temperature corrosion evaluation method introduced in this study, the surface and cross-sectional corrosion of the specimens were confirmed by using scanning electron microscopy and energy-dispersive X-ray analysis. Based on these analysis results, it was found that the corrosion resistance of the commercial heat exchanger materials increases as the content of chrome and nickel in the composition increases. Additionally, it was found that the corrosion phenomenon is rapidly accelerated as the surface temperature increases. Finally, the replacement period (lifetime) of the heat exchanger tubes under each condition could be inferred through this study.

Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.