• Title/Summary/Keyword: SEM-EDS techniques

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Oxide Nanolayers Grown on New Ternary Ti Based Alloy Surface by Galvanic Anodizing-Characteristics and Anticorrosive Properties

  • Calderon Moreno, J.M.;Drob, P.;Vasilescu, C.;Drob, S.I.;Popa, M.;Vasilescu, E.
    • Corrosion Science and Technology
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    • v.16 no.5
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    • pp.257-264
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    • 2017
  • Film of new Ti-15Zr-5Nb alloy formed during galvanic anodizing in orthophosphoric acid solution was characterized by optical microscope, scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and Raman micro-spectroscopy. Its anticorrosive properties were determined by electrochemical techniques. The film had a layer with nanotube-like porosity with diameters in 500-1000 nm range. The nano layer contained significant amounts of P and O as well as alloying element. Additionally, Raman micro-spectroscopy identified oxygen as oxygen ion in $TiO_2$ anatase and phosphorous as $P_2O_7{^{4-}}$ ion in phosphotitanate compound. All potentiodynamic polarization curves in artificial Carter-Brugirard saliva with pH values (pH= 3.96, 7.84, and 9.11) depending on the addition of 0.05M NaF revealed nobler behavior of anodized alloy and higher polarization resistance indicating the film is thicker and more compact nanolayer. Lower corrosion rates of the anodized alloy reduced toxicity due to less released ions into saliva. Bigger curvature radii in Nyquist plot and higher phase angle in Bode plot for the anodized alloy ascertain a thicker, more protective, insulating nanolayer existing on the anodized alloy. Additionally, ESI results indicate anodized film consists of an inner, compact, barrier, layer and an outer, less protective, porous layer.

Methane Dry Reforming over Ru/CeO2 catalysts (Ru/CeO2 촉매를 이용한 메탄 건식 개질)

  • HIEN, NGUYEN THI BICH;JEON, MINA;RIDWAN, MUHAMMAD;TAMARANY, RIZCKY;YOON, CHANG WON
    • Transactions of the Korean hydrogen and new energy society
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    • v.26 no.3
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    • pp.221-226
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    • 2015
  • Ru catalysts supported on $CeO_2$ were synthesized by an impregnation method and characterized by numerous analytical techniques including X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), transmission electron microscopy (TEM), and scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS). Upon utilization of these catalysts for methane dry reforming with a $CH_4/CO_2$ ratio of 1:1 at different temperatures ranging from 550 to $750^{\circ}C$, the $Ru/CeO_2$ catalysts have shown to be active. In particular, Ru(0.55wt%) supported on $CeO_2$ (1) prepared by a hydrothermal method exhibited excellent activity with the conversion of > 75% at $750^{\circ}C$. In addition, the catalyst also proved to be highly stable for at least 47 h without catalyst deactivation under the dry reforming conditions.

Formation and Structure of $CaO-P_2O_5-SiO_2$ Glasses ($CaO-P_2O_5-SiO_2$계 유리의 형성 및 구조)

  • 조정식;김철영
    • Journal of the Korean Ceramic Society
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    • v.29 no.9
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    • pp.729-738
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    • 1992
  • The glass formation and structural change with the glass compositions were investigated in the CaO-P2O5-SiO2 system with less than 40 wt% of P2O5. The glass formation range was determined by XRD, SEM and EDS techniques for water quenched specimens. The structural analyses were made for binary CaO-SiO2 glasses and ternary CaO-P2O5-SiO2 glasses by using FT-IR and Raman spectroscopy. The glass formation was affected by CaO/SiO2 mole ratio, P2O5 content and primary crystalline phase. The stable glass formation range was found when the transformed CaO/SiO2 mole ratio (new factor derived from structural changes) was in the range of 0.72~1.15 with less than 10 mol% of P2O5. The structural analyses of CaO-SiO2 glasses indicated that as the CaO/SiO2 ratio was increased, the nonbridging oxygens in the structural unit of the glasses were increased. With addition of P2O5 to CaO-SiO2 glasses, the P2O5 enhanced the polymerization of [SiO4] tetrahedra unit in CaO-SiO2 glasses, which contained a large portion of nonbridging oxygen. The phosphate eliminated nonbridging oxygens from silicate species, forcing polymerization of silicate structures and produced in [PO4] monomer in glasses. When added P2O5 was kept constant, the structural change with various CaO/SiO2 ratio was very similar to that of CaO-SiO2 glasses.

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Si and Mg Coatings on the Hydroxyapatite Film Formed Ti-29Nb-xHf Alloys by Plasma Electrolyte Oxidation

  • Park, Seon-Yeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.152-152
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    • 2017
  • Titanium and its alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element,such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}$-stabilizer and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Therefore, in this study, Si and Mg coatings on the hydroxyapatite film formed Ti-29Nb-xHf alloys by plasma electrolyte oxidation has been investigated using several experimental techniques. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. The electrolyte was Si and Mg ions containing calcium acetate monohydrate + calcium glycerophosphate at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

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Analysis of Surface Contaminants and Removal Techniques on Three-story Stone Pagoda at the West of Gameunsaji Site (감은사지서삼층석탑의 표면오염물 분석과 제거기술)

  • Kim, Sa-Dug;Lee, Tae-Jong;Kim, Da-Ram;Han, Min-Su
    • Journal of Conservation Science
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    • v.26 no.2
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    • pp.203-211
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    • 2010
  • Analytic research on the surface pollutant of the three storied-pagoda at the west of Gameunsaji site as well as studies of previous wet cleaning cases was undertaken in order to decide cleaning method for removing inorganic pollutants. The status of pollutant was examined by naked eye observation, SEM-EDS, XRD. Then it was compared and categorized through qualitive and quantitative analysis. The result showed that the surface pollutants consisted of iron compounds or sulfur compounds and it was crystallized in the form of circle, oval, needle, etc. Result, Low-pressure rotating vortex process cleaning, with which particular matters are sprayed in swirl, is considered to be the best method to remove the pollutants.

Characteristic Evaluation of Anodic Film Depending on the Concentration of Sodium Silicate in the Electrolyte Anodized AZ31B Magnesium Alloy (전해액 중 Sodium silicate의 농도에 따라 양극 산화된 AZ31B 마그네슘 합금 양극 피막의 특성 평가)

  • Lee, Dong-Kil;Kim, Yong-Hwan;Park, Hyun;Jung, Uoo-Chang;Chung, Won-Sub
    • Journal of the Korean institute of surface engineering
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    • v.42 no.3
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    • pp.109-115
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    • 2009
  • Magnesium is one of the lightest metals, and magnesium alloys have excellent physical and mechanical properties such as high stiffness/weight ratios, good castability, good vibration and shock absorption. However their poor corrosion resistance, wear resistance, hardness and so on, have limited their application. To improve these defects, many techniques are developed. Micro arc oxidation(MAO) is a one of the surface treatments under anodic oxidation in which ceramic coating is directly formed on the surface of magnesium alloy. In this study, the characteristics of anodic film were examined after coating the AZ31B magnesium alloy through the MAO process. MAO was carried out in potassium hydroxide, potassium fluoride, and various concentration of sodium silicate in electrolyte. The morphology and chemical composition of the coating layer were characterized by SEM, XRD, EPMA and EDS. The hardness of anodic films was measured by micro-vickers hardness tester. As a result, the morphology and composition of anodic film were changed by concentration of sodium silicate. Thickness and Si composition of anodic film was increased with increasing concentration of sodium silicate in electrolyte. The hardness of anodic film was highly increased when the concentration of sodium silicate was above 40 g/l in electrolyte.

Improvement in Grade of Sericite Ore by Dry Beneficiation (건식정제에 의한 견운모광의 품위향상연구)

  • Cho, Keon-Joon;Kim, Yun-Jong;Park, Hyun-Hae;Cho, Sung-Baek
    • Korean Journal of Materials Research
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    • v.19 no.4
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    • pp.212-219
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    • 2009
  • A study on the dry beneficiation of sericite occurring in the Daehyun Mine of the Republic of Korea region as performed by applying selective grinding and air classification techniques. Quartz and sericite occurred in the raw ore as major components. The results of liberation using a ball mill and an impact mill showed that the contents of $R_2O$ were increased while $SiO_2$ was decreased in proportion to decreasing particle size. According to the XRD, XRF analysis and the EDS of SEM analysis, the ball mill gave a better grade product in $R_2O$ content than the impact mill when the particle size was the same. When the raw ore was ground by the impact mill with arotor speed 57.6 m/sec and then followed by 15,000rpm classification using an air classifier, the chemical composition of the over flowed product was 49.65wt% $SiO_2$, 32.15wt% $Al_2O_3$, 0.13wt% $Fe_2O_3$, 10.37wt% $K_2O$, and 0.14wt% $Na_2O$. This result indicates that the $R_2O$ contents were increased by 49.5% compared to that of the raw ore. From these results described above, it is suggested that hard mineral such as Quartz little ground by selective grinding using impact mill whereas soft mineral such as sericite easily ground to small size. As a result of that hard minerals can be easily removed from the finely ground sericite by air classification and the $R_2O$ grade of thus obtained concentrate was improved to higher than 10wt% which can be used for ceramics raw materials.

Effects of different surface treatments on the shear bond strength of veneering ceramic materials to zirconia

  • Abdullah, Adil Othman;Hui, Yu;Sun, Xudong;Pollington, Sarah;Muhammed, Fenik Kaml;Liu, Yi
    • The Journal of Advanced Prosthodontics
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    • v.11 no.1
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    • pp.65-74
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    • 2019
  • PURPOSE. To evaluate and compare the effect of different materials and techniques on the shear bond strength of veneering ceramic materials to zirconia. MATERIALS AND METHODS. 136 sintered zirconia cubes were prepared and randomly divided into four study groups according to corresponding methods of surface treatment and materials: GLN (grinding followed by laser scanning using Noritake Cerabien ZR), SLN (sandblasting followed by laser scanning using Noritake Cerabien ZR), GLV (grinding followed by laser scanning using VITA VM 9), and SLV (sandblasting followed by laser scanning using VITA VM 9). Spraying technique was performed to coat the core. Profilometer, SEM, XRD, EDS, universal testing machine, and stereomicroscope were used to record surface roughness Ra, surface morphology, phase transformation, elemental compositions, shear bond strength SBS values, and failure types, respectively. Specimens were investigated in unaged (not immersed in artificial saliva) and aged (stored in artificial saliva for a month) conditions to evaluate SBS values. RESULTS. Grinding and GLN as first and second surface treatments provided satisfactory Ra values in both conditions ($1.05{\pm}0.24{\mu}m$, $1.30{\pm}0.21{\mu}m$) compared to sandblasting and other groups (P<.05). The group GLN showed the highest SBS values in both conditions ($30.97{\pm}3.12MPa$, $29.09{\pm}4.17MPa$), while group SLV recorded the lowest ($23.96{\pm}3.60MPa$, $22.95{\pm}3.68Mpa$) (P<.05). Sandblasting showed phase transformation from t-m. Mixed failure type was the commonest among all groups. CONCLUSION. GLN showed to be a reliable method which provided satisfactory bond strength between the veneer ceramic and zirconia. This method might preserve the integrity of fixed dental crowns.

Experimental design approach for ultra-fast nickel removal by novel bio-nanocomposite material

  • Ince, Olcay K.;Aydogdu, Burcu;Alp, Hevidar;Ince, Muharrem
    • Advances in nano research
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    • v.10 no.1
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    • pp.77-90
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    • 2021
  • In the present study, novel chitosan coated magnetic magnetite (Fe3O4) nanoparticles were successfully biosynthesized from mushroom, Agaricus campestris, extract. The obtained bio-nanocomposite material was used to investigate ultra-fast and highly efficient for removal of Ni2+ ions in a fixed-bed column. Chitosan was treated as polyelectrolyte complex with Fe3O4 nanoparticles and a Fungal Bio-Nanocomposite Material (FBNM) was derived. The FBNM was characterized by using X-Ray Diffractometer (XRD), Scanning Electron Microscopy-Energy Dispersive X-Ray Spectroscopy (SEM-EDS), Fourier Transform Infrared spectra (FTIR) and Thermogravimetric Analysis (TGA) techniques and under varied experimental conditions. The influence of some important operating conditions including pH, flow rate and initial Ni2+ concentration on the uptake of Ni2+ solution was also optimized using a synthetic water sample. A Central Composite Design (CCD) combined with Response Surface Modeling (RSM) was carried out to maximize Ni2+ removal using FBNM for adsorption process. A regression model was derived using CCD to predict the responses and analysis of variance (ANOVA) and lack of fit test was used to check model adequacy. It was observed that the quadratic model, which was controlled and proposed, was originated from experimental design data. The FBNM maximum adsorption capacity was determined as 59.8 mg g-1. Finally, developed method was applied to soft drinks to determine Ni2+ levels. Reusability of FBNM was tested, and the adsorption and desorption capacities were not affected after eight cycles. The paper suggests that the FBNM is a promising recyclable nanoadsorbent for the removal of Ni2+ from various soft drinks.

Enhancement of FeCrAl-ODS steels through optimised SPS parameters and addition of novel nano-oxide formers

  • A. Meza;E. Macia;M. Serrano;C. Merten;U. Gaitzsch;T. Weissgarber;M. Campos
    • Nuclear Engineering and Technology
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    • v.56 no.7
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    • pp.2584-2594
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    • 2024
  • A novel approach to incorporating oxide formers into ferritic ODS production has been developed using the co-precipitation technique. This method enables the tailored design of complex nano-oxides, integrated during Mechanical Alloying (MA) and precipitated during Spark Plasma Sintering (SPS) consolidation. Findings illustrate that co-precipitation effectively produces nano-powders with customised compositions, enriching Y, Ti, and Zr in the ferritic grade to condition subsequent oxide precipitation. While the addition of Y-Ti-Zr-O nano-oxides did not prevent the formation of Y-Al-O and Al-containing nano-oxides, these were refined thanks to the presence of well-dispersed Zr. Additionally, the Spark Plasma Sintering (SPS) parameters were optimised to tailor the bimodal grain size distribution of the ODS steels, aiming for favourable strength-to-ductility ratios. Comprehensive microstructural analyses were performed using SEM, EDS, EBSD, and TEM techniques, alongside mechanical assessments involving microtensile tests conducted at room temperature and small punch tests carried out at room temperature, 300 ℃, and 500 ℃. The outcomes yielded promising findings, showcasing similar or better performance with conventionally manufactured ODS steels. This reinforces the effectiveness and success of this innovative approach.