• Title/Summary/Keyword: EDS solution

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Microfluidic Assisted Synthesis of Ag-ZnO Nanocomposites for Enhanced Photocatalytic Activity (광촉매 성능 강화를 위한 미세유체공정 기반 Ag-ZnO 나노복합체 합성)

  • Ko, Jae-Rak;Jun, Ho Young;Choi, Chang-Ho
    • Clean Technology
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    • v.27 no.4
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    • pp.291-296
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    • 2021
  • Recently, there has been increasing demand for advancing photocatalytic techniques that are capable of the efficient removal of organic pollutants in water. TiO2, a representative photocatalytic material, has been commonly used as an effective photocatalyst, but it is rather expensive and an alternative is required that will fulfill the requirements of both high performing photocatalytic activities and cost-effectiveness. In this work, ZnO, which is more cost effective than TiO2, was synthesized by using a microreactor-assisted nanomaterials (MAN) process. The process enabled a continuous production of ZnO nanoparticles (NPs) with a flower-like structure with high uniformity. In order to resolve the limited light absorption of ZnO arising from its large band gap, Ag NPs were uniformly decorated on the flower-like ZnO surface by using the MAN process. The plasmonic effect of Ag NPs led to a broadening of the absorption range toward visible wavelengths. Ag NPs also helped inhibit the electron-hole recombination by drawing electrons generated from the light absorption of the flower-like ZnO NPs. As a result, the Ag-ZnO nanocomposites showed improved photocatalytic activities compared with the flower-like ZnO NPs. The photocatalytic activities were evaluated through the degradation of methylene blue (MB) solution. Scanning electron microscopy (SEM), x-ray diffraction (XRD), and energy-dispersive x-ray spectroscopy (EDS) confirmed the successful synthesis of Ag-ZnO nanocomposites with high uniformity. Ag-ZnO nanocomposites synthesized via the MAN process offer the potential for cost-effective and scalable production of next-generation photocatalytic materials.

Ni/Au Electroless Plating for Solder Bump Formation in Flip Chip (Flip Chip의 Solder Bump 형성을 위한 Ni/Au 무전해 도금 공정 연구)

  • Jo, Min-Gyo;O, Mu-Hyeong;Lee, Won-Hae;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.6 no.7
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    • pp.700-708
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    • 1996
  • Electroless plating technique was utilized to flip chip bonding to improve surface mount characteristics. Each step of plating procedure was studied in terms pf pH, plating temperature and plating time. Al patterned 4 inch Si wafers were used as substrstes and zincate was used as an activation solution. Heat treatment was carried out for all the specimens in the temperature range from room temperature to $400^{\circ}C$ for $30^{\circ}C$ minutes in a vacuum furnace. Homogeneous distribution of Zn particles of size was obtained by the zincate treatment with pH 13 ~ 13.5, solution concentration of 15 ~ 25% at room temperature. The plating rates for both Ni-P and Au electroless plating steps increased with increasing the plating temperature and pH. The main crystallization planes of the plated Au were found to be (111) a pH 7 and (200) and (111) at pH 9 independent of the annealing temperature.

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Identification of Sorption Characteristics of Cesium for the Improved Coal Mine Drainage Treated Sludge (CMDS) by the Addition of Na and S (석탄광산배수처리슬러지에 Na와 S를 첨가하여 개량한 흡착제의 세슘 흡착 특성 규명)

  • Soyoung Jeon;Danu Kim;Jeonghyeon Byeon;Daehyun Shin;Minjune Yang;Minhee Lee
    • Economic and Environmental Geology
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    • v.56 no.2
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    • pp.125-138
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    • 2023
  • Most of previous cesium (Cs) sorbents have limitations on the treatment in the large-scale water system having low Cs concentration and high ion strength. In this study, the new Cs sorbent that is eco-friendly and has a high Cs removal efficiency was developed by improving the coal mine drainage treated sludge (hereafter 'CMDS') with the addition of Na and S. The sludge produced through the treatment process for the mine drainage originating from the abandoned coal mine was used as the primary material for developing the new Cs sorbent because of its high Ca and Fe contents. The CMDS was improved by adding Na and S during the heat treatment process (hereafter 'Na-S-CMDS' for the developed sorbent in this study). Laboratory experiments and the sorption model studies were performed to evaluate the Cs sorption capacity and to understand the Cs sorption mechanisms of the Na-S-CMDS. The physicochemical and mineralogical properties of the Na-S-CMDS were also investigated through various analyses, such as XRF, XRD, SEM/EDS, XPS, etc. From results of batch sorption experiments, the Na-S-CMDS showed the fast sorption rate (in equilibrium within few hours) and the very high Cs removal efficiency (> 90.0%) even at the low Cs concentration in solution (< 0.5 mg/L). The experimental results were well fitted to the Langmuir isotherm model, suggesting the mostly monolayer coverage sorption of the Cs on the Na-S-CMDS. The Cs sorption kinetic model studies supported that the Cs sorption tendency of the Na-S-CMDS was similar to the pseudo-second-order model curve and more complicated chemical sorption process could occur rather than the simple physical adsorption. Results of XRF and XRD analyses for the Na-S-CMDS after the Cs sorption showed that the Na content clearly decreased in the Na-S-CMDS and the erdite (NaFeS2·2(H2O)) was disappeared, suggesting that the active ion exchange between Na+ and Cs+ occurred on the Na-S-CMDS during the Cs sorption process. From results of the XPS analysis, the strong interaction between Cs and S in Na-S-CMDS was investigated and the high Cs sorption capacity was resulted from the binding between Cs and S (or S-complex). Results from this study supported that the Na-S-CMDS has an outstanding potential to remove the Cs from radioactive contaminated water systems such as seawater and groundwater, which have high ion strength but low Cs concentration.

Synthesis of Garnet in the Ca-Ce-Gd-Zr-Fe-O System (Ca-Gd-Ce-Zr-Fe-O계에서의 석류석 합성 연구)

  • Chae Soo-Chun;Jang Young-Nam;Bae In-Kook;Yudintsev S.V.
    • Economic and Environmental Geology
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    • v.38 no.2 s.171
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    • pp.187-196
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    • 2005
  • Structural sites which cations can occupy in garnet structure are centers of the tetrahedron, octahedron, and distorted cube sharing edges with the tetrahedron and octahedron. Among them, the size of cation occuping at tetrahedral site (the center of tetrahedron) is closely related with the size of a unit cell of garnet. Accordingly, garnet containing iron with relative large ionic radii in tetrahedral site can be considered as a promising matrix for the immobilization of the elements with large ionic radii, such as actinides in radioactive wastes. We synthesized several garnets with the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$, and studied their properties and phase relations under various conditions. Mixed samples were fabricated in a pellet form under a pressure of $200{\~}400{\cal}kg/{\cal}cm^2$ and were sintered in the temperature range of $1100\~1400^{\circ}C$ in air and under oxygen atmospheres. Phase identification and chemical analysis of synthesized samples were conducted by XRD and SEM/EDS. In results, garnet was obtained as the main phase at $1300^{\circ}C$, an optimum condition in this system, even though some minor phases like perovskite and unknown phase were included. The compositions of garnet and perovskite synthesized from the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$ were ranged $[Ca_{l.2-1.8}Gd_{0.9-1.4}Ce_{0.3-0.5}]^{VIII}[Zr_{0.8-1.3}Fe_{0.7-1.2}]^{VI}[Fe_{2.9-3.1}]^{IV}O_{12}$ and $Ca_{0.1-0.5}Gd_{0.0-0.8}Ce_{0.1-0.5}\;Zr_{0.0-0.2}Fe_{0.9-1.1}O_3$, respectively. Ca content was exceeded and Ce content was depleted in the 8-coordinated site, comparing to the initial batch composition. This phenomena was closely related to the content of Zr and Fe in the 6-coordinated site.

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.

A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.239-240
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    • 2008
  • As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

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Dry reforming of Propane to Syngas over Ni-CeO2/γ-Al2O3 Catalysts in a Packed-bed Plasma Reactor (충전층 플라즈마 반응기에서 Ni-CeO2/γ-Al2O3 촉매를 이용한 프로페인-합성 가스 건식 개질)

  • Sultana, Lamia;Rahman, Md. Shahinur;Sudhakaran, M.S.P.;Hossain, Md. Mokter;Mok, Young Sun
    • Clean Technology
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    • v.25 no.1
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    • pp.81-90
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    • 2019
  • A dielectric barrier discharge (DBD) plasma reactor packed with $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was used for the dry ($CO_2$) reforming of propane (DRP) to improve the production of syngas (a mixture of $H_2$ and CO) and the catalyst stability. The plasma-catalytic DRP was carried out with either thermally or plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst at a $C_3H_8/CO_2$ ratio of 1/3 and a total feed gas flow rate of $300mL\;min^{-1}$. The catalytic activities associated with the DRP were evaluated in the range of $500{\sim}600^{\circ}C$. Following the calcination in ambient air, the ${\gamma}-Al_2O_3$ impregnated with the precursor solution ($Ni(NO_3)_2$ and $Ce(NO_3)_2$) was subjected to reduction in an $H_2/Ar$ atmosphere to prepare $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst. The characteristics of the catalysts were examined using X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectrometry (EDS), temperature programmed reduction ($H_2-TPR$), temperature programmed desorption ($H_2-TPD$, $CO_2-TPD$), temperature programmed oxidation (TPO), and Raman spectroscopy. The investigation revealed that the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst exhibited superior catalytic activity for the production of syngas, compared to the thermally reduced catalyst. Besides, the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was found to show long-term catalytic stability with respect to coke resistance that is main concern regarding the DRP process.