• Title/Summary/Keyword: energy-dispersive x-ray spectroscopy (eds)

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Study on Ti-doped LiNi0.6Co0.2Mn0.2O2 Cathode Materials for High Stability Lithium Ion Batteries (고안정성 리튬이온전지 양극활물질용 Ti 치환형 LiNi0.6Co0.2Mn0.2O2 연구)

  • Jeon, Young Hee;Lim, Soo A
    • Journal of the Korean Electrochemical Society
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    • v.24 no.4
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    • pp.120-132
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    • 2021
  • Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO2, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi0.6Co0.2Mn0.2O2, precursor Ni0.6Co0.2Mn0.2-x(OH)2/xTiO2 was prepared using a nanosized TiO2 suspension type source for uniform Ti substitution in the precursor. It was mixed with Li2CO3, and after heating, the cathode active material LiNi0.6Co0.2Mn0.2-xTixO2 was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.

Biosorption of Heavy Metal in Aqueous Solution by Heavy Metal Tolerant Microorganism Isolated from Heavy Metal Contaminated Soil (중금속으로 오염된 토양에서 분리한 중금속 내성 미생물의 수용액내 중금속 흡착)

  • Kim, Sung-Un;Choi, Ik-Won;Seo, Dong-Cheol;Han, Myung-Hoon;Kang, Byung-Hwa;Heo, Jong-Soo;Shon, Bo-Kyoon;Cho, Ju-Sik
    • Korean Journal of Environmental Agriculture
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    • v.24 no.4
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    • pp.379-385
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    • 2005
  • This study was conducted to find out a useful bioremediation technology for heavy metal contaminated soil and water. We isolated strain CPB from heavy metal contaminated soil and evaluated the tolerance level and adsorption capacity of strain CPB to heavy metals (Strain is not determined yet). Strain CPB showed variable tolerance limit to different kinds heavy metal or concentrations of heavy metals. The growth of strain CPB was significantly inhibited by mixed heavy metals (Cd+Cu+Pb+Zn) than that of by single heavy metal. Strain CPB showed high binding capacity with Pb (Pb>Cd>Cu>Zn). In general, strain CPB showed high uptake of heavy metals such as Pb, Cd and Cu. It was observed that the capacity of heavy metal uptake from mixture of heavy metals was reduced in comparison with single heavy metal treatment. But total contents of heavy metal bound with cell in mixed heavy metal showed higher than in single heavy metal treatment. Heavy metal adsorption in cells was affected by several external factors, such as temperature and pH etc.. The optimum temperature and pH of the adsorption of heavy metal into cells were ca. $25{\sim}35^{\circ}C$ and pH ca. $5{\sim}7$, respectively. A large number of the electron dense particles were found mainly on the cell wall and cell membrane fractions, which was determined by transmission electron microscope. Energy dispersive X-ray spectroscopy revealed that the electron dense particles were the heavy metal complexes the substances binding with heavy metals.

Copper Accumulation in Cells of Copper-Tolerant Bacteria, Pseudomonas stutzeri (구리 내성균(Pseudomonas stutzeri)의 균체내 구리 축적특성)

  • Cho, Ju-Sik;Han, Mun-Gyu;Lee, Hong-Jae;Heo, Jong-Soo
    • Korean Journal of Environmental Agriculture
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    • v.16 no.1
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    • pp.48-54
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    • 1997
  • This study was performed to develop the biological treatment technology of wastewater polluted with heavy metals. The copper-tolerant bacteria, Pseudomonas stutzeri which possessed the ability to accumulate copper, was isolated from mine wastewaters polluted with various heavy metals. The characteristics of copper accumulation in the cells and the recovery of the copper from the cells accumulating zinc, were investigated. Removal rate of copper from the solution containing 100mg/l of copper by copper-tolerant bacteria was more than 78% at 2 days after inoculation with the cells. A large number of the electron-dense granules were found mainly on the cell wall and cell membrane fractions, when determined by transmission electron microscopy. Energy dispersive X-ray spectroscopy revealed that the electron-dense granules were copper complex with the substances binding copper. The copper accumulated into the cells was not desorbed by deistilled water, but more than 80% of the copper accumulated was desorbed by 0.1M-EDTA solution. The residues of the cells after combustion at $550^{\circ}C$ amounted to about 23.2% of the dry weight of the cells. EDS analysis showed that residues were relatively pure copper compound containing more than 78.4% of copper.

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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.

A Case of Enterolithiasis in a Grant's Zebra (Equus burchelli boehmi) and Analysis of the Enterolith (그랜트얼룩말에서 발생한 장결석증과 결석의 분석)

  • Kim, Ji-Yong;Kim, Yang-Beom;Kwon, Soo-Whan;Lee, Wang-Hee;Choi, Yoon-Ju;Lee, Won-Jung;Yoo, Han-Sang;Shin, Nam-Shik
    • Journal of Veterinary Clinics
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    • v.27 no.1
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    • pp.93-96
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    • 2010
  • We describe a case of enterolithiasis in an eight-year-old male Grant's zebra (Equus burchelli boehmi) that died after a 10-day history of depression, anorexia, dehydration and colic. On necropsy, an enterolith was discovered at the conjunction of the descending colon and the rectum. The spherical enterolith weighed 1,660 g and was $13.5cm{\times}8cm$ in size. According to scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS), the nidus consisted primarily of $SiO_2$ with outer layers of magnesium and phosphate. The formation of enteroliths is closely related to diet. We suggest that this captive zebra's diet, which consisted primarily of alfalfa hay with mineral supplements, was the cause of enterolithiasis in this case. This is the first report of enterolithiasis in a captive equid in Korea. Our findings provide information valuable for the development of dietary guidelines to prevent enterolithiasis in captive wild equids.

Development of a Hydrogen Peroxide Sensor Based on Palladium and Copper Electroplated Laser Induced Graphene Electrode (PdCu를 전기 도금한 레이저 유도 그래핀 전극 기반의 과산화수소 측정 센서 개발)

  • Park, Daehan;Han, Ji-Hoon;Kim, Taeheon;Pak, Jungho
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.67 no.12
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    • pp.1626-1632
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    • 2018
  • In this paper, we describe the fabrication and characterization of a hydrogen peroxide ($H_2O_2$) sensor based on palladium and copper (PdCu) electroplated laser induced graphene (LIG) electrodes. $CO_2$ laser was used to form LIG electrodes on a PI film. This fabrication method allows simple control of the LIG electrode size and shape. The PdCu was electrochemically deposited on the LIG electrodes to improve the electrocatalytic reaction with $H_2O_2$. The electrochemical performance of this sensor was evaluated in terms of selectivity, sensitivity, and linearity. The physical characterization of this sensor was conducted using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), which confirmed that PdCu was formed on the laser induced graphene electrode. In order to increase the sensor sensitivity, the Pd:Cu ratio of the electroplated PdCu was varied to five different values and the condition of highest amperometric current at an identical of $H_2O_2$ concentration was chosen among them. The resulting amperometric current was highest when the ratio of Pd:Cu was 7:3 and this Pd;Cu ratio was employed in the sensor fabrication. The fabricated PdCu/LIG electrode based $H_2O_2$ sensor exhibited a sensitivity of $139.4{\mu}A/mM{\cdot}cm^2$, a broad linear range between 0 mM and 16 mM of $H_2O_2$ concentrations at applied potential of -0.15 V, and high reproducibility (RSD = 2.6%). The selectivity of the fabricated sensors was also evaluated by applying ascorbic acid, glucose, and lactose separately onto the sensor in order to see if the sensor ourput is affected by one of them and the sensor output was not affected. In conclusion, the proposed PdCu/LIG electrode based $H_2O_2$ sensor seems to be suitable $H_2O_2$ sensor in various applications.

A Non-enzymatic Hydrogen Peroxide Sensor Based on CuO Nanoparticles/polyaniline on Flexible CNT Fiber Electrode (CuO Nanoparticles/polyaniline/CNT fiber 유연 전극 기반의 H2O2 검출용 비효소적 전기화학 센서)

  • Min-Jung Song
    • Korean Chemical Engineering Research
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    • v.61 no.2
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    • pp.196-201
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    • 2023
  • In this study, a CNT fiber flexible electrode grafted with CuO nanoparticles (CuO NPs) and polyaniline (PANI) was developed and applied to a nonenzymatic electrochemical sensor for H2O2 detection. CuO NPs/PANI/CNT fiber electrode was fabricated through the synthesis and deposition of PANI and CuO NPs on the CNT fiber surface using an electrochemical method. Surface morphology and elemental composition of the CuO NPs/PANI/CNT fiber electrode were characterized by scanning electron microscope with energy dispersive X-ray spectrometry. And its electrochemical characteristics were investigated by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and chronoamperometry (CA). Compared with a bare CNT fiber as a control group, the CuO NPs/PANI/CNT fiber electrode showed a 4.78-fold increase in effective surface area and a 8.33-fold decrease in electron transfer resistance, which leads to excellent electrochemical properties such as a good electrical conductivity and an efficient electron transfer. These improved characteristics were due to the synergistic effect through the grafting of CNT fiber, PANI and CuO NPs. As a result, this electrode enhanced the H2O2 sensing performance.

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.

모재/중간층/박막의 H/E ratio 구배에 따른 Cr계 경질 박막의 기계적 특성에 관한 연구

  • Kim, Hoe-Geun;Song, Myeon-Gyu;Lee, Sang-Yul
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.135-135
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    • 2018
  • 천이금속 질화물 코팅은 우수한 기계적 특성들로 인해 공구 코팅으로 많이 사용 되어왔다. 그 중에서도 특히 Cr계 경질 코팅은 높은 경도와 낮은 표면조도, 우수한 마찰특성 등 뛰어난 기계적 특성을 나타내므로 공구 코팅으로의 적용 가능성이 크다. 그러나 최근 공구산업의 발전으로 인해 공구가 더욱 가혹한 환경에서 사용됨에 따라, 공구의 수명을 향상시키고 보호하기 위해 코팅의 높은 밀착력이 요구되고 있으며, 모재와 코팅 사이에 중간층을 합성함으로써 공구의 밀착력을 향상시키는 연구가 활발히 진행되고 있다. 이전 연구에서 모재/중간층/코팅간의 경도와 탄성계수 비율(H/E ratio)의 구배가 코팅의 밀착력에 큰 영향을 미치는 것으로 확인되었다. 그러므로, WC 모재와 Cr계 코팅의 중간값의 H/E ratio를 갖는 중간층의 합성을 통해 코팅의 밀착력을 향상시킬 수 있을 것으로 판단된다. 본 연구에서는, 코팅의 밀착력을 향상시키기 위해 다양한 중간층을 증착한 CrZrN, CrAlN 코팅을 비대칭 마그네트론 스퍼터링 장비를 이용하여 합성하였다. 모재로는 디스크 형상의 WC-6wt.%Co 시편을 사용하였고 Cr, Zr, Si, Al single 타겟을 이용하여 Cr, CrN, CrZrN, CrZrSiN 등의 중간층이 증착된 코팅을 합성했다. 코팅의 합금상, 경도 및 탄성계수, 미세조직 및 조성, 표면 조도을 확인하기 위해 X-ray diffractometer (XRD), Fischer scope, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), atomic force microscopy를 사용하였고, 코팅의 밀착 특성을 분석하기 위해 scratch tester와 optical microscopy (OM)를 이용하였다. 코팅의 내열성을 확인하기 위해 코팅을 furnace에 넣어 공기중에서 500, 600, 700, 800, 900, $1,000^{\circ}C$로 30분 동안 annealing 한 후에 nano-indentation을 사용하여 경도를 측정하였다. CrZrN 및 CrAlN 코팅을 나노 인덴테이션으로 분석한 결과, 모든 코팅의 경도(33.4-35.8 GPa)와 탄성계수(384.1-391.4 GPa)는 중간층의 종류에 상관없이 비슷한 값을 보인 것으로 확인됐다. 그러나, 코팅의 마찰계수는 중간층의 종류에 따라 다른 값을 보였다. CrZrN 코팅의 경우 CrN 합금상 중간층을 갖을 때 가장 낮은 값을 보였으며, CrAlN 코팅의 경우 CrN/CrZrSiN 중간층을 증착하였을때 마찰계수는 0.34로 CrZrN 중간층을 증착하였을 때(0.41)에 비해 낮은 값을 보였다. 또한, 코팅의 마모율 및 마모폭도 비슷한 경향을 보인 것으로 보아, CrN/CrZrSiN 중간층을 합성한 CrAlN 코팅의 내마모성이 상대적으로 우수한 것으로 판단된다. 코팅의 밀착력의 경우도 마찰계수와 비슷한 경향을 보였다. 이것은 중간층의 H/E ratio가 코팅의 내마모성에 미치는 영향에 의한 결과로 사료된다. H/E ratio는 파단시의 최대 탄성 변형율로써, 모재/중간층/코팅의 H/E ratio 구배에 따라 코팅 내의 응력의 완화 정도가 변하게 된다. WC 모재 (H/E=0.040)와 CrAlN 코팅(H/E=0.089) 사이에서 CrN, CrZrSiN 중간층의 H/E ratio는 각각 0.076, 0.083으로 모재/중간층/코팅의 H/E ratio 구배가 점차 증가함을 확인 할 수 있었고, 일정 응력이 지속적으로 가해지면서 진행되는 마모시험중에 CrN과 CrZrSiN 중간층이 WC와 CrAlN 코팅 사이에서 코팅 내부의 응력구배를 완화시키는 역할을 함으로써 CrAlN 코팅의 내마모성이 향상된 것으로 판단된다. 모든 코팅을 열처리 후 경도 분석 결과, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅은 $1,000^{\circ}C$까지 약 28GPa의 높은 경도를 유지한 것으로 확인 되었고, 이는 CrZrSiN 중간층 내에 존재하는 SiNx 비정질상의 우수한 내산화성에 의한 결과로 판단된다.

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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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