• Title/Summary/Keyword: Raman Spectroscopy

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A Study on the Vanadium Oxide Thin Films as Cathode for Lithium Ion Battery Deposited by RF Magnetron Sputtering (RF 마그네트론 스퍼터링으로 증착된 리튬 이온 이차전지 양극용 바나듐 옥사이드 박막에 관한 연구)

  • Jang, Ki-June;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.6
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    • pp.80-85
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    • 2019
  • Vanadium dioxide is a well-known metal-insulator phase transition material. Lots of researches of vanadium redox flow batteries have been researched as large scale energy storage system. In this study, vanadium oxide($VO_x$) thin films were applied to cathode for lithium ion battery. The $VO_x$ thin films were deposited on Si substrate($SiO_2$ layer of 300 nm thickness was formed on Si wafer via thermal oxidation process), quartz substrate by RF magnetron sputter system for 60 minutes at $500^{\circ}C$ with different RF powers. The surface morphology of as-deposited $VO_x$ thin films was characterized by field-emission scanning electron microscopy. The crystallographic property was confirmed by Raman spectroscopy. The optical properties were characterized by UV-visible spectrophotometer. The coin cell lithium-ion battery of CR2032 was fabricated with cathode material of $VO_x$ thin films on Cu foil. Electrochemical property of the coin cell was investigated by electrochemical analyzer. As the results, as increased of RF power, grain size of as-deposited $VO_x$ thin films was increased. As-deposited thin films exhibit $VO_2$ phase with RF power of 200 W above. The transmittance of as-deposited $VO_x$ films exhibits different values for different crystalline phase. The cyclic performance of $VO_x$ films exhibits higher values for large surface area and mixed crystalline phase.

Effect of Temperature on Growth of Tin Oxide Nanostructures (산화주석 나노구조물의 성장에서 기판 온도의 효과)

  • Kim, Mee-Ree;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.497-502
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    • 2019
  • Metal oxide nanostructures are promising materials for advanced applications, such as high sensitive gas sensors, and high capacitance lithium-ion batteries. In this study, tin oxide (SnO) nanostructures were grown on a Si wafer substrate using a two-zone horizontal furnace system for a various substrate temperatures. The raw material of tin dioxide ($SnO_2$) powder was vaporized at $1070^{\circ}C$ in an alumina crucible. High purity Ar gas, as a carrier gas, was flown with a flow rate of 1000 standard cubic centimeters per minute. The SnO nanostructures were grown on a Si substrate at $350{\sim}450^{\circ}C$ under 545 Pa for 30 minutes. The surface morphology of the as-grown SnO nanostructures on Si substrate was characterized by field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). Raman spectroscopy was used to confirm the phase of the as-grown SnO nanostructures. As the results, the as-grown tin oxide nanostructures exhibited a pure tin monoxide phase. As the substrate temperature was increased from $350^{\circ}C$ to $424^{\circ}C$, the thickness and grain size of the SnO nanostructures were increased. The SnO nanostructures grown at $450^{\circ}C$ exhibited complex polycrystalline structures, whereas the SnO nanostructures grown at $350^{\circ}C$ to $424^{\circ}C$ exhibited simple grain structures parallel to the substrate.

Effect of Substrate Temperature and Growth Duration on Palladium Oxide Nanostructures (팔라듐 옥사이드 나노구조물의 성장에서 기판 온도와 성장 시간의 효과)

  • Kim, Jong-Il;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.458-463
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    • 2019
  • Palladium (Pd) is widely used as a catalyst and noxious gas sensing materials. Especially, various researches of Pd based hydrogen gas sensor have been studied due to the noble property, Pd can be adsorbed hydrogen up to 900 times its own volume. In this study, palladium oxide (PdO) nanostructures were grown on Si substrate ($SiO_2(300nm)/Si$) for 3 to 5 hours at $230^{\circ}C{\sim}440^{\circ}C$ using thermal chemical vapor deposition system. Pd powder (source material) was vaporized at $950^{\circ}C$ and high purity Ar gas (carrier gas) was flown with the 200 sccm. The surface morphology of as-grown PdO nanostructures were characterized by field-emission scanning electron microscopy(FE-SEM). The crystallographic properties were confirmed by Raman spectroscopy. As the results, the as-grown nanostructures exhibit PdO phase. The nano-cube structures of PdO were synthesized at specific substrate temperatures and specific growth duration. Especially, PdO nano-cube structrures were uniformly grown at $370^{\circ}C$ for growth duration of 5 hours. The PdO nano-cube structures are attributed to vapor-liquid-solid process. The nano-cube structures of PdO on graphene nanosheet can be applied to fabricate of high sensitivity hydrogen gas sensor.

Growth of Tin Dioxide Nanostructures on Chemically Synthesized Graphene Nanosheets (화학적으로 합성된 그래핀 나노시트 위에서의 이산화주석 나노구조물의 성장)

  • Kim, Jong-IL;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.5
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    • pp.81-86
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    • 2019
  • Metal oxide/graphene composites have been known as promising functional materials for advanced applications such as high sensitivity gas sensor, and high capacitive secondary battery. In this study, tin dioxide ($SnO_2$) nanostructures were grown on chemically synthesized graphene nanosheets using a two-zone horizontal furnace system. The large area graphene nanosheets were synthesized on Cu foil by thermal chemical vapor deposition system with the methane and hydrogen gas. Chemically synthesized graphene nanosheets were transferred on cleaned $SiO_2$(300 nm)/Si substrate using the PMMA. The $SnO_2$ nanostuctures were grown on graphene nanosheets at $424^{\circ}C$ under 3.1 Torr for 3 hours. Raman spectroscopy was used to estimate the quality of as-synthesized graphene nanosheets and to confirm the phase of as-grown $SnO_2$ nanostructures. The surface morphology of as-grown $SnO_2$ nanostructures on graphene nanosheets was characterized by field-emission scanning electron microscopy (FE-SEM). As the results, the synthesized graphene nanosheets are bi-layers graphene nanosheets, and as-grown tin oxide nanostructures exhibit tin dioxide phase. The morphology of $SnO_2$ nanostructures on graphene nanosheets exhibits complex nanostructures, whereas the surface morphology of $SnO_2$ nanostructures on $SiO_2$(300 nm)/Si substrate exhibits simply nano-dots. The complex nanostructures of $SnO_2$ on graphene nanosheets are attributed to functional groups on graphene surface.

The Effect of Heat Treatment Condition on the Mechanical Properties of oxi-PAN Based Carbon Fiber (Oxi-PAN 섬유를 기반으로 제조한 탄소섬유의 탄화 조건에 따른 구조 및 물성의 변화)

  • Choi, Kyeong Hun;Heo, So Jeong;Hwang, Sang-Ha;Bae, Soo Bin;Lee, Hyung Ik;Chae, Han Gi
    • Composites Research
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    • v.31 no.6
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    • pp.385-391
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    • 2018
  • In this study, carbon fibers were fabricated via carbonization of oxidized polyacrylonitrile (oxi-PAN) under different carbonization conditions. Carbonization of oxi-PAN fiber was performed under four different temperature (1300, 1400, 1500, $1600^{\circ}C$) with four different fiber tensions (14, 25, 35, 45 MPa). Effect of carbonization process on the structural development and mechanical properties of carbon fiber were characterized by single filament fiber tensile test and Raman spectroscopy. A clear correlation exists between the Raman spectrum and the tensile modulus of carbon fiber and effect of carbonization temperature on the tensile modulus showed increased tendency only at higher fiber tension (${\geq}25MPa$) while tensile strength showed decreased or random tendency. Therefore, it may be concluded that the optimization of carbonization temperature of oxi-PAN fiber also requires optimization of fiber tension.

Aqueous Boron Adsorption on Carbonized Nanofibers Prepared from Electrospun Polyacrylonitrile(PAN) Mats (전기방사 후 탄소화된 폴리아크릴로니트릴(PAN) 나노섬유의 수용액 중 붕소 흡착)

  • Hong, So Hee;Han, Sun-Gie;Kim, Su Young;Won, Yong Sun
    • Clean Technology
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    • v.28 no.3
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    • pp.210-217
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    • 2022
  • Boron(B) is a rare resource used for various purposes such as glass, semiconductor materials, gunpowder, rocket fuel, etc. However, Korea depends entirely on imports for boron. Considering the global boron reserves and its current production rate, boron will be depleted on earth in 50 years. Thus, a process including proper adsorbent materials recovering boron from seawater is demanded. This research proposed carbonized nanofibers prepared from electrospun PAN(polyacrylonitrile) mats as promising materials to adsorb boron in aqueous solution. First, the mechanism of boron adsorption on carbonized nanofibers was investigated by DFT(density functional method)-based molecular modeling and the calculated energetics demonstrated that the boron chemisorption on the nitrogen-doped graphene surface by a two-step dehydration is possible with viable activation energies. Then, the electrospun PAN mats were stabilized in air and then carbonized in an argon atmosphere before being immersed in the boric acid aqueous solution. Analytically, SEM(scanning electron microscopy) and Raman measurements were employed to confirm whether the electrospinning and carbonization of PAN mats proceeded successfully. Then, XPS(X-ray photoelectron spectroscopy) peak analysis showed whether the intended nitrogen-doped carbon nanofiber surface was formed and boron was properly adsorbed on nanofibers. Those results demonstrated that the carbonized nanofibers prepared from electrospun PAN mats could be feasible adsorbents for boron recovery in seawater.

Research on Physicochemical Properties of Graphene Oxide (GO) and Reduced Graphene Oxide (R-GO) (그래핀 옥사이드(Graphen Oxide, GO)와 환원 그래핀의 (Reduced graphe oxide, R-GO)의 물리화학적 특성 연구)

  • Moo-Sun Kim;Ho-Yong Lee;Sung-Woong Choi
    • Composites Research
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    • v.36 no.3
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    • pp.167-172
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    • 2023
  • The manufacturing technology of composite material is applicable with filler characteristics maintaining low cost, flexibility, and easy process to develope the various functional composite materials. To realize functional composites, various researches on the high performance of composite materials using graphene as a filler is being actively conducted. In this study, physical and chemical properties were investigated using graphene to improve high functional properties. Graphene oxide (GO) was prepared using graphane nanoplatelet (GNP), and reduced graphene oxide (R-GO) was formed by reducing GO. The physical properties of GO and R-GO were analyzed, and the reliability of the manufactured method was reviewed by comparing that of GNP results. As a result of analysis by Raman spectroscopy, in the case of R-GO, it was confirmed that the intensity of D-peak and G-peak decreased compared to GO, and an increase of 0.08 was observed through the ratio of ID/IG. For the FTIR results, GO and RGO has a repeating C-C and C=C connection structure unlike GNP. GO and R-GO show clear peaks for C-O bond, C=C bond, C=O bond, and O-H bonding. As a result of X-ray diffraction analysis, GNP showed a wide diffraction peak at 25.86° of (002) plane characteristics, whereas GO and R-GO showed peaks corresponding to (001) and (100) planes. It was also found that the interlayer distance of GO increased by about 2.6 times compared to GNP.

Controlling the Work Functions of Graphene by Functionalizing the Surface of $SiO_2$ Substrates with Self-assembled Monolayers

  • Jo, Ju-Mi;Kim, Yu-Seok;Cha, Myeong-Jun;Lee, Su-Il;Jeong, Sang-Hui;Song, U-Seok;Kim, Seong-Hwan;Jeon, Seung-Han;Park, Jong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.400-401
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    • 2012
  • 그래핀(Graphene)은 열 전도도가 높고 전자 이동도(200 000 cm2V-1s-1)가 우수한 전기적 특성을 가지고 있어 전계 효과 트랜지스터(Field effect transistor; FET), 유기 전자 소자(Organic electronic device)와 광전자 소자(Optoelectronic device) 같은 반도체 소자에 응용 가능하다. 그러나 에너지 밴드 갭이 없기 때문에 소자의 전기적 특성이 제한되는 단점이 있다. 최근에는 아크 방출(Arc discharge method), 화학적 기상 증착법(Chemical vapor deposition; CVD), 이온-조사법(Ion-irradiation) 등을 이용한 이종원자(Hetero atom)도핑과 화학적 처리를 이용한 기능화(Functionalization) 등의 방법으로 그래핀을 도핑 후 에너지 밴드 갭을 형성시키는 연구 결과들이 보고된 바 있다. 그러나 이러한 방법들은 표면이 균일하지 않고, 그래핀에 많은 결함들이 발생한다는 단점이 있다. 이러한 단점을 극복하기 위해 자가조립 단층막(Self-assembled monolayers; SAMs)을 이용하여 이산화규소(Silicon oxide; SiO2) 기판을 기능화한 후 그 위에 그래핀을 전사하면 그래핀의 일함수를 쉽게 조절하여 소자의 전기적 특성을 최적화할 수 있다. SAMs는 그래핀과 SiO2 사이에 부착된 매우 얇고 안정적인 층으로 사용된 물질의 특성에 따라 운반자 농도나 도핑 유형, 디락 점(Dirac point)으로부터의 페르미 에너지 준위(Fermi energy level)를 조절할 수 있다[1-3]. 본 연구에서는 SAMs한 기판을 이용하여 그래핀의 도핑 효과를 확인하였다. CVD를 이용하여 균일한 그래핀을 합성하였고, 기판을 3-Aminopropyltriethoxysilane (APTES)와 Borane-Ammonia(Borazane)을 이용하여 각각 아민 기(Amine group; -NH2)와 보론 나이트라이드(Boron Nitride; BN)로 기능화한 후, 그 위에 합성한 그래핀을 전사하였다. 기판 위에 NH2와 BN이 SAMs 형태로 존재하는 것을 접촉각 측정(Contact angle measurement)을 통해 확인하였고, 그 결과 NH2와 BN에 의해 그래핀에 도핑 효과가 나타난 것을 라만 분광법(Raman spectroscopy)과 X-선 광전자 분광법(X-ray photoelectron spectroscopy: XPS)을 이용하여 확인하였다. 본 연구 결과는 안정적이면서 패턴이 가능하기 때문에 그래핀을 기반으로 하는 반도체 소자에 적용 가능할 것이라 예상된다.

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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.

Characterization of Nitrogen-Doped $TiO_2$ Thin Films Prepared by Metalorganic Chemical Vapor Deposition (유기금속 화학 기상증착법으로 실리콘 기판위에 증착된 질소치환 $TiO_2$ 박막의 특성분석)

  • 이동헌;조용수;이월인;이전국;정형진
    • Journal of the Korean Ceramic Society
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    • v.31 no.12
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    • pp.1577-1587
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    • 1994
  • TiO2 thin films with the substitution of oxygen with nitrogen were deposited on silicon substrate by metalorganic chemical vapor deposition (MOCVD) using Ti(OCH(CH3)2)4 (titanium tetraisopropoxide, TTIP) and N2O as source materials. X-ray diffraction (XRD) results indicated that the crystal structure of the deposited thin films was anatase TiO2 with only (101) plane observed at the deposition temperatures of 36$0^{\circ}C$ and 38$0^{\circ}C$, and with (101) and (200) plane at above 40$0^{\circ}C$. Raman spectroscopic results indicated that the crystal structure was anatase TiO2 in accordance with the XRD results without any rutile, fcc TiN, or hcp TiN structure. No fundamental difference was observed with temperature increase, but the peak intensity at 194.5 cm-1 increased with strong intensity at 143.0 cm-1 for all samples. The crystalline size of the films varied from 49.2 nm to 63.9 nm with increasing temperature as determined by slow-scan XRD experiments. The refractive index of the films increased from 2.40 to 2.55 as temperature increased. X-ray photoelectron spectroscopy (XPS) study showed only Ti 2s, Ti 2p, C 1s, O 1s and O 2s peaks at the surface of the film. The composition of the surface was estimated to be TiO1.98 from the quatitative analysis. In the bulk of the film Ti 2s, Ti 2p, O 1s, O 2s, N 1s and N 2s were detected, and Ti-N bonding was observed due to the substitution of oxygen with nitrogen. A satellite structure was observed in the Ti 2p due to the Ti-N bonding, and the composition of titanium nitride was determined to be about TiN1.0 from the position of the binding energy of Ti-N 2p3/2 and the quatitative analysis. The spectrum of Ti 2p energy level could be the sum of a 4, 5, or 6 Gaussian curve reconstruction, and the case of the sum of the 6 Gaussian curve reconstruction was physically most meaningful. From the results of Auger electron spectroscopy (AES), it was known that the composition was not varied significantly throughout the whole thickness of the film, and silicon oxide was not observed at the interface between the film and the substrate. The composition of the film was possible (TiO2)1-x.(TiN)x or TiO2-2xNx and in this experimental condition x was found to be about 0.21-0.16.

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