• Title/Summary/Keyword: SEM-EDX analysis

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Evaluation of Raw and Calcined Eggshell for Removal of Cd2+ from Aqueous Solution

  • Kim, Youngjung;Yoo, Yerim;Kim, Min Gyeong;Choi, Jong-Ha;Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.64 no.5
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    • pp.249-258
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    • 2020
  • The potential use of egg shell and calcined egg shell as adsorbent was evaluated and compared to remove Cd2+ from aqueous solution. The samples were characterized using Thermogravimetry and Differential Thermal Analysis (TG/DTA), Scanning Electron Microscope (SEM), X-ray Diffractometer (XRD), Energy Dispersive X-ray Spectrometer (EDX) and BET Surface Analyzer. The batch-type adsorption experiment was conducted by varying diverse variables such as contact time, pH, initial Cd2+ concentrations and adsorbent dosage. The results showed that, under the initial Cd2+ concentrations ranged from 25 to 200 mg g-1, the removal efficiencies of Cd2+ by egg shell powder (ESP) were decreased steadily from 96.72% to 22.89% with increase in the initial Cd2+ concentration at 2.5 g of dosage and 8 h of contact time. However, on the contrary to this, calcined egg shell powder (CESP) showed removal efficiencies above 99% regardless of initial Cd2+ concentration. The difference in the adsorption behavior of Cd2+ may be explained due to the different pH values of ESP and CESP in solution. Cd2+ seems to be efficiently removed from aqueous solution by using the CESP with a basicity nature of around pH 12. It was also observed that an optimum dosage of ESP and CESP for nearly complete removal of Cd2+ from aqueous solution is approximately 5.0 g and 1.0 g, respectively. Consequently, Cd2+ is more favorably adsorbed on CESP than ESP in the studied conditions. Adsorption data were applied by the pseudo-first-order and pseudo-second-order kinetics models and Freundlich and Langmuir isotherm models, respectively. With regard to adsorption kinetics tests, the pseudo-second-order kinetics was more suitable for ESP and CESP. The adsorption pattern of Cd2+ by ESP was better fitted to Langmuir isotherm model. However, by contrast with ESP, CESP was described by Freundlich isotherm model well.

Effects of acid-treatment conditions on the surface properties of the RBM treated titanium implants (산-처리 조건이 RBM처리한 티타늄 임플란트의 표면 특성에 주는 영향)

  • Lee, Han-Ah;Seok, Soohwang;Lee, Sang-Hyeok;Lim, Bum-Soon
    • Korean Journal of Dental Materials
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    • v.45 no.4
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    • pp.257-274
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    • 2018
  • The purpose of this study was to evaluate the effect of acid-treatment conditions on the surface properties of the RBM (Resorbable Blast Media) treated titanium. Disk typed cp-titanium specimens were prepared and RBM treatments was performed with calcium phosphate ceramic powder. Acid solution was mixed using HCl, $H_2SO_4$ and deionized water with 4 different volume fraction. The RBM treated titanium was acid treated with different acid solutions at 3 different temperatures and for 3 different periods. After acid-treatments, samples were cleaned with 1 % Solujet solution for 30 min and deionized water for 30 min using ultrasonic cleanser, then dried in the electrical oven ($37^{\circ}C$). Weight of samples before and after acid-treatment were measured using electric balance. Surface roughness was estimated using a confocal laser scanning microscopy, crystal phase in the surface of sample was analyzed using X-ray diffractometer. Surface morphology and components were evaluated using Scanning Electron Microscope (SEM) with Energy Dispersive X-ray spectroscopy (EDX) and X-ray Photoemission Spectroscopy (XPS). Values of the weight changes and surface roughness were statistically analyzed using Tukey-multiple comparison test (p=0.05). Weight change after acid treatments were significantly increased with increasing the concentration of $H_2SO_4$ and temperature of acid-solution. Acid-treatment conditions (concentration of $H_2SO_4$, temperature and time) did not produce consistent effects on the surface roughness, it showed the scattered results. From XRD analysis, formation of titanium hydrides in the titanium surface were observed in all specimens treated with acid-solutions. From XPS analysis, thin titanium oxide layer in the acid-treated specimens could be evaluated. Acid solution with $90^{\circ}C$ showed the strong effect on the titanium surface, it should be treated with caution to avoid the over-etching process.

Microbial Leaching of Iron from Magnetite (미생물을 이용한 자철석으로부터 철 침출에 관한 연구)

  • Roh, Yul;Oh, Jong-Min;Seo, Yong-Jae;Jang, Hee-Dong
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.4 s.50
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    • pp.265-275
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    • 2006
  • It is in its infancy to use bacteria as a novel biotechnology for leaching precious and heavy metals from raw materials. The objective of this study was to investigate biogeochemical processes of iron leaching from magnetite reduction by iron-reducing bacteria isolated from intertidal flat sediments, southwestern part of Korea. Microbial leaching experiments were performed using commercial magnetite, Aldrich magnetite, in well-defined mediums with and without bacteria. Water soluble Fe production was determined by ICP analysis of bioleached samples in comparison to uninoculated controls, and the resulting precipitated solids were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The extent of iron leaching from magnetite in the aerobic conditions (Fe = 107 ppm) was higher than that in the anaerobic environments (Fe = 94 ppm). In the anaerobic conditions, Fe(III) in commercial magnetite was also reduced to Fe(II), but no secondary mineral phases were observed. Amorphous iron oxides formed in the medium under aerobic conditions where there was sufficient supply of oxygen from the atmosphere. SEM observation suggests that the reduction process involves dissolution-precipitation mechanisms as opposed to solid state conversion of magnetite to amorphous iron oxides. The ability of bacteria to leach soluble iron and precipitate amorphous iron oxides from crystalline magnetite could have significant implications for biogeochemical processes in sediments where Fe(III) in magnetite plays an important role in the largest pool of electron acceptor as well as the tool as a novel biotechnology for leaching precious and heavy metals from raw materials.

A.C. Impedance Properties of HA/Ti Compound Layer coated Ti-30Ta-(3~15)Nb Alloys (Ti-30Ta-(3~15)Nb 합금에 HA/Ti 복합 코팅한 표면의 교류임피던스 특성)

  • Jeong, Y.H.;Lee, H.J.;Moong, Y.P;Park, G.H.;Jang, S.H.;Son, M.K.;Choe, H.C.
    • Journal of the Korean institute of surface engineering
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    • v.41 no.5
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    • pp.181-188
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    • 2008
  • A.C. impedance properties of HA/Ti compound layer coated Ti-30Ta-($3{\sim}15$)Nb alloys have been studied by electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10 and 15 wt% Nb were manufactured by the vacuum furnace system. And then specimen was homogenized at $1000^{\circ}C$ for 24 hrs. The sample was cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The non-coated and coated morphology of Ti alloy were analyzed by X-ray diffractometer (XRD), energy X-ray dispersive spectroscopy (EDX) and filed emission scanning electron microscope (FE-SEM). The corrosion behaviors were investigated using A.C. impedance test (PARSTAT 2273, USA) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Ti-30Ta-($3{\sim}15\;wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and $\beta$ phase peak was predominantly appeared in the case of increasingly Nb contents. The microstructures of Ti alloy were transformed from needle-like structure to equiaxed structure as Nb content increased. From the analysis of coating surface, HA/Ti composite surface uniformed coating layer with 750 nm thickness. The growth directions of film were (211), (112), (300) and (202) for HA/Ti composite coating on the surface after heat treatment at $550^{\circ}C$, whereas, the growth direction of film was (110) for Ti coating. The polarization resistance ($R_p$) of HA/Ti composite coated Ti-alloys were higher than those of the Ti and HA coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

Development of Metal Loaded Activated Carbon Fiber for Eliminating Targeted VOCs Originated from Solvent(II) (특정용제 Target 형 활성금속첨착 활성탄소섬유의 개발(II))

  • Choi, Kang-Yong;Kim, Kwang-Su;Kim, Tae-Won;Jun, Min-Kee;Park, Hea-Kyung
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.7
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    • pp.472-478
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    • 2013
  • Cu and Cr as a base metal and Pt, Pd as a supportive metal were selected for improving adsorption capacity of activated carbon fiber in eliminating especially targeted VOCs. Preparing variables such as metal loading, loading temperature, loading hours and kinds of loaded metals were changed. Properties measurement was carried out by SEM (scanning electron microscope), XRF (x-ray fluorescence analysis) and EDX (Energy Dispersive X-ray spectrometer) and adsorption capacity evaluation were also performed by gas analyzer. Under this study, the adsorption capacity of complex metal loaded activated carbon fiber was improved positively than that of single metal loaded activated carbon fiber. And we found that the best conditions for metal loading were 5 hours loading time at $100^{\circ}C$ and the adsorption capacity was enhanced almost double compared with other condition based activated carbon fiber. Cu-Cr-Pt-Pd loaded activated carbon fiber showed the best adsorption capacity. Also we confirmed that more than 0.5 second is necessary for adsorbate diffusion and adsorption over activated carbon fiber.

Sol-Gel Synthesis, Crystal Structure, Magnetic and Optical Properties in ZnCo2O3 Oxide

  • Das, Bidhu Bhusan;Barman, Bittesh
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.453-458
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    • 2019
  • Synthesis of ZnCo2O3 oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo2O3. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O2 in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at giso ~2.230 and giso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co2+(3d7) in the oxide. DC conductivity value of 2.875 ×10-8 S/cm indicates very weakly semiconducting nature of ZnCo2O3 at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions 4T1g(4F)→2Eg(2G), 4T1g(4F)→4T1g(4P), 4T1g(4F)→4A2g(4F), 4T1g(4F)→4T2g(4F), respectively in octahedral ligand field around Co2+ ions. Direct band gap energy, Eg~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo2O3.

Experimental Study on Engineering Properties of Concrete Using Fluosilicates Based Composite (규불화염계 복합 조성물을 혼입한 콘크리트의 공학적 특성에 관한 실험적 연구)

  • Yang Il-Seung;Yun Hyun-Do;Kim Do-Su;Khil Bae-Su;Han Seung-Gu
    • Journal of the Korea Concrete Institute
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    • v.17 no.5 s.89
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    • pp.769-774
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    • 2005
  • Fluosilicic acid(H2SiF6) is recovered as an aqueous solution which absorbs $SiF_4$ produced from the manufacturing of industrial-graded H3PO4 or HF. Generally, fluosilicates are the salts produced by the reaction of H2SiF6 and metal salts. Addition of fluosilicates to cement endows odd properties through unique chemical reaction with the fresh and hardened cement. This study was performed to know mechanical properties and watertightness using fluosilicates based composite made from fluosilicates and other compounds. Mix proportions for experiments were modulated at 0.45 of water to cement ratio and $0.0-2.0\%$ of adding ratio of fluosilicates based composite. Evaluation for mechanical properties of concrete was conducted to know fresh state of concrete, hardening state of concrete, and watertightness. Evaluation for watertightness of concrete was carried out permeability, absorption test and porosity analysis. In addition. Scanning Electron Microscopy(SEM) and Energy Dispersive X-Ray(EDX) used for investigating micro-structure and atomic component distributed in hardened concrete. It is ascertained that characteristics of mechanical properties and watertightness was more improved than non-added because of packing role of fluosilicates based composite and pozzolanic reaction of soluble $SiO_2$. Also, concrete added fluosilicates based composite had a tendency to delay setting time and only $0.5\%$ addition of fluosilicates based composite delayed 150 minutes compared with non-added.

Preparation of Metal Hydrides Using Chemical Synthesis and Hydriding Kinetics (화학적 합성법에 의한 금속수소화물의 제조 및 수소화 속도론적 연구)

  • Lee, Yun Sung;Oh, Jae Wan;Moon, Sung Sik;Nahm, Kee Suk
    • Applied Chemistry for Engineering
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    • v.9 no.2
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    • pp.255-260
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    • 1998
  • Metal hydrides, $LaNi_5$ and $LaNi_{4.5}Al_{0.5}$, were prepared using chemical synthetic method, and their physical properties were examined using various analytic techniques such as TGA, XRD, SEM and EDX. The activation of the chemically prepared $LaNi_5$ and $LaNi_{4.5}Al_{0.5}$ was achieved by two hydriding/dehydriding cycles only. The miasurements of P-C-T curves revealed that 6 and 5.5 hydrogen atoms were stored in LaNi5and $LaNi_{4.5}Al_{0.5}$, respectively. The hydriding reaction rated for $LaNi_{4.5}Al_{0.5}$ were measured by the method of initial rates. It was found that the shrinking unreacted core model could be applied for the analysis of hydriding kinetics of $LaNi_5$. The rate controlling step of this reaction was the dissociative chemisorption of hydrogen molecules on the surface of $LaNi_5$. The activation energy was $9.506kcal/mol-H_2$. The rates measured in the temperature range from 273 to 343K and in pressure difference ($P_o-P_{eq}$) range form 0.25 to 0.66atm could be expressed as the following equation ; $\frac{dX}{dt}=4.636(P_o-P_{eq})$ exp($\frac{-9506}{RT}$).

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DEVELOPMENT OF SN BASED MULTI COMPONENT SOLDER BALLS WITH CD CORE FOR BGA PACKAGE

  • Sakatani, Shigeaki;Kohara, Yasuhiro;Uenishi, Keisuke;Kobayashi, Kojiro F.;Yamamoto, Masaharu
    • Proceedings of the KWS Conference
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    • 2002.10a
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    • pp.450-455
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    • 2002
  • Cu-cored Sn-Ag solder balls were fabricated by coating pure Sn and Ag on Cu balls. The melting behavior and the solderability of the BGA joint with the Ni/Au coated Cu pad were investigated and were compared with those of the commercial Sn-Ag and Sn-Ag-Cu balls. DSC analyses clarified the melting of Cu-cored solders to start at a rather low temperature, the eutectic temperature of Sn-Ag-Cu. It was ascribed to the diffusion of Cu and Ag into Sn plating during the heating process. After reflow soldering the microstructures of the solder and of the interfacial layer between the solder and the Cu pad were analyzed with SEM and EPMA. By EDX analysis, formation of a eutectic microstructure composing of $\beta$-Sn, Ag$_3$Sn, ad Cu$_{6}$Sn$_{5}$ phases was confirmed in the solder, and the η'-(Au, Co, Cu, Ni)$_{6}$Sn$_{5}$ reaction layer was found to form at the interface between the solder and the Cu pad. By conducting shear tests, it was found that the BGA joint using Cu-cored solder ball could prevent the degradation of joint strength during aging at 423K because of the slower growth me of η'-(Au, Co, Cu, Ni)$_{6}$Sn$_{5}$ reaction layer formed at the solder, pad interface. Furthermore, Cu-cored multi-component Sn-Ag-Bi balls were fabricated by sequentially coating the binary Sn-Ag and Sn-Bi solders on Cu balls. The reflow property of these solder balls was investigated. Melting of these solder balls was clarified to start at the almost same temperature as that of Sn-2Ag-0.75Cu-3Bi solder. A microstructure composing of (Sn), Ag$_3$Sn, Bi and Cu$_{6}$Sn$_{5}$ phases was found to form in the solder ball, and a reaction layer containing primarily η'-(Au, Co, Cu, Ni)$_{6}$Sn$_{5}$ was found at the interface with Ni/Au coated Cu pad after reflow soldering. By conducting shear test, it was found that the BGA joints using this Cu-core solder balls hardly degraded their joint shear strength during aging at 423K due to the slower growth rate of the η'-(Au, Cu, Ni)$_{6}$Sn$_{5}$ reaction layer at the solder/pad interface.he solder/pad interface.

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Properties of Capacity on Carbon Electrode in EC : MA Electrolyte II. Effect of Additives on Initial Irreversible Capacity (EC : MA 혼합전해질에서 카본 전극의 용량 특성 II. 초기 비가역 용량에 대한 첨가제의 효과)

  • Park, Dong-Won;Kim, Woo-Seong;Son, Dong-Un;Choi, Yong-Kook
    • Applied Chemistry for Engineering
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    • v.17 no.6
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    • pp.575-579
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    • 2006
  • Solid electrolyte interface is formed on a carbon electrode used as an anode in Li-ion battery, which can be of $Li^{+}$ intercalation/deintercalation during the first cycle. The passivation film formed by a solvent decomposition during the initial charge process affects cell performance and it was one of the main reason of an initial irreversible capacity. This paper describes the use, for the first time, of $Li_2CO_3$ as the additive for the formation of a passivation film on the carbon surface to suppress the initial irreversible reaction. Chronopotentiometry, cyclic voltammetry, and impedance spectroscopy were used to investigate the effects of the $Li_{2}CO_{3}$ additive. Scanning electron microscopy, energy dispersive X-ray analysis, and X-ray diffraction were also used to monitor changes in the surface morphology and composition of the passivation film formed by solvent decomposition and the precipitation of $Li_{2}CO_{3}$. The addition of $Li_{2}CO_{3}$ to a solution of 1 M $LiPF_{6}$/EC:MA (1:3, v/v) resulted in a decrease in the initial irreversible capacity and it was due to the suppression of the solvent decomposition on the electrode surface.