• Title/Summary/Keyword: 라만 분광 분석

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Phase Behavior and Structural Analyses of the THF + H2 Binary Clathrate Hydrate (THF + H2 이성분계 크러스레이트 하이드레이트의 상거동 및 구조 분석)

  • Cha, Jong-Ho;Park, Youngjune;Cha, Min-Jun;Yeon, Sun-Hwa;Lee, Huen
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1095-1099
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    • 2008
  • In this study, we investigated that hydrate formation and phase behavior of the $THF+H_2$ binary clathrate hydrates. In order to confirm the binary clathrate hydrate formation we employed the Raman and NMR spectroscopies that are known to be quite powerful tools, particularly for examining the cage occupancy pattern of guest molecules. In addition, we traced the P-T profiles from clathrate hydrate formation and dissociation process, which made it possible for the resulting phase equilibrium boundary to be clearly established. In the binary clathrate hydrate matrix we further identified that the relatively large THF molecules can only occupy the large $5^{12}6^4$ cavities, while the small $H_2$ molecules are entrapped in the empty $5^{12}$ cavities in structure-II, making the hydrate to be stable above 273 K even at relatively low pressure condition. Considering that pure $H_2$ hydrate can be produced at the extreme pressures higher that 1,000 bar, we can conclude that the water-soluble second guest inclusion induces $H_2$ storage and transportation to be readily achievable under much milder conditions.

Automatic Selection of Optimal Parameter for Baseline Correction using Asymmetrically Reweighted Penalized Least Squares (Asymmetrically Reweighted Penalized Least Squares을 이용한 기준선 보정에서 최적 매개변수 자동 선택 방법)

  • Park, Aaron;Baek, Sung-June;Park, Jun-Qyu;Seo, Yu-Gyung;Won, Yonggwan
    • Journal of the Institute of Electronics and Information Engineers
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    • v.53 no.3
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    • pp.124-131
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    • 2016
  • Baseline correction is very important due to influence on performance of spectral analysis in application of spectroscopy. Baseline is often estimated by parameter selection using visual inspection on analyte spectrum. It is a highly subjective procedure and can be tedious work especially with a large number of data. For these reasons, it is an objective and automatic procedure is necessary to select optimal parameter value for baseline correction. Asymmetrically reweighted penalized least squares (arPLS) based on penalized least squares was proposed for baseline correction in our previous study. The method uses a new weighting scheme based on the generalized logistic function. In this study, we present an automatic selection of optimal parameter for baseline correction using arPLS. The method computes fitness and smoothness values of fitted baseline within available range of parameters and then selects optimal parameter when the sum of normalized fitness and smoothness gets minimum. According to the experimental results using simulated data with varying baselines, sloping, curved and doubly curved baseline, and real Raman spectra, we confirmed that the proposed method can be effectively applied to optimal parameter selection for baseline correction using arPLS.

Catalytic Behavior of Ni/CexZr1-xO2-Al2O3 Catalysts for Methane Steam Reforming: The CexZr1-xO2 Addition Effect on Water Activation (메탄 습식 개질 반응용 Ni/CexZr1-xO2-Al2O3 촉매의 반응 특성: CexZr1-xO2 첨가에 의한 물 활성화 효과)

  • Haewon Jung;Huy Nguyen-Phu;Mingyan Wang;Sang Yoon Kim;Eun Woo Shin
    • Korean Chemical Engineering Research
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    • v.61 no.3
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    • pp.479-486
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    • 2023
  • In this study, we investigated the effect of the CexZr1-xO2 (CZ) addition onto Ni/Al2O3 catalysts on the catalytic performance in methane steam reforming. In the reaction results, the CZ-added Ni/Al2O3 catalyst showed higher CH4 conversion and H2 yield under the same reaction conditions than Ni/Al2O3. From the characterization data, the two catalysts had similar support porosity and Ni dispersion, confirming that the two properties could not determine the catalytic performance. However, the oxygen vacancy over the CZ-added Ni/Al2O3 catalyst induced an efficient steam activation at low reaction temperatures, resulting in an increase in the catalytic activity and H2 yield.

Electrical response of tungsten diselenide to the adsorption of trinitrotoluene molecules (폭발물 감지 시스템 개발을 위한 TNT 분자 흡착에 대한 WSe2 소자의 전기적 반응 특성 평가)

  • Chan Hwi Kim;Suyeon Cho;Hyeongtae Kim;Won Joo Lee;Jun Hong Park
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.6
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    • pp.255-260
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    • 2023
  • As demanding the detection of explosive molecules, it is required to develop rapidly and precisely responsive sensors with ultra-high sensitivity. Since two-dimensional semiconductors have an atomically thin body nature where mobile carriers accumulate, the abrupt modulation carrier in the thin body channel can be expected. To investigate the effectiveness of WSe2 semiconductor materials as a detection material for TNT (Trinitrotoluene) explosives, WSe2 was synthesized using thermal chemical vapor deposition, and afterward, WSe2 FETs (Field Effect Transistors) were fabricated using standard photo-lithograph processes. Raman Spectrum and FT-IR (Fourier-transform infrared) spectroscopy reveal that the adsorption of TNT molecules induces the structural transition of WSe2 crystalline. The electrical properties before and after adsorption of TNT molecules on the WSe2 surface were compared; as -50 V was applied as the back gate bias, 0.02 μA was recorded in the bare state, and the drain current increased to 0.41 μA with a dropping 0.6% (w/v) TNT while maintaining the p-type behavior. Afterward, the electrical characteristics were additionally evaluated by comparing the carrier mobility, hysteresis, and on/off ratio. Consequently, the present report provides the milestone for developing ultra-sensitive sensors with rapid response and high precision.

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.

Synthesis of Nanostructured Si Coatings by Hybrid Plasma-Particle Accelerating Impact Deposition (HP-PAID) and their Characterization (하이브리드 플라즈마 입자가속 충격퇴적(Hybrid Plasma - Particle Accelerating Impact Deposition, HP-PAID) 프로세스에 의한 Si 나노구조 코팅층의 제조 및 특성평가)

  • 이형직;권혁병;정해경;장성식;윤상옥;이형복;이홍림
    • Journal of the Korean Ceramic Society
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    • v.40 no.12
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    • pp.1202-1207
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    • 2003
  • Using a recently developed Hybric Plasma-Particle Accelerating Impact Deposition (HP-PAID) process, synthesis of nanostructured silicon coatings has been investigated by injecting vapor-phase TEOS (tetraethosysilane, (C$_2$H$\_$5/O)$_4$Si) into an Ar hybrid plasma. The plasma jet with reactants was expanded through nozzle into a deposition chamber, with the pressure dropping from 700 to 10 torr. Ultrafine particles accelerated in the free jet downstream of the nozzle, deposited by an inertial impaction onto a temperature controlled substrate. By using this process, nanostructured amorphous silicon coatings with grain size smaller than 10 nm could be synthesized. These samples were annealed in an Ar and crystallized at 900$^{\circ}C$ for 30 min. TEM analysis showed that the annealed coatings were also composed of nanoparticles smaller than 10 nm, which showed a good consistency that the average grain size of 7 nm was also estimated from a peak shift of 2.39 cm$\^$-1/ and Full Width at Half Maximum (FWHM) 5.92 cm$\^$-1/ of Raman analysis. The noteworthy is that a strong PL peak at 398 nm was also obtained for this sample, which indicates that the deposited coatings also contained 3∼4 nm nanostructured grains.

Synthesis of High-Quality Monolayer Graphene on Copper foil by Chemical Vapor Deposition

  • Lee, Su-Il;Kim, Yu-Seok;Song, U-Seok;Jo, Ju-Mi;Kim, Seong-Hwan;Park, Jong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.351-352
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    • 2011
  • 그래핀(Graphene)은 2차원 평면구조의 $sp^2$ 탄소 결합으로 이루어진 물질이다. 일반적으로 그래핀은 탄소 원자 한층 정도의 얇은 두께를 가지면서 강철의 100배 이상 높은 강도, 다이아몬드보다 2배 이상 뛰어난 열 전도성, 그리고 규소보다 100배 이상 빠른 전자이동도 등의 매우 우수한 특성을 지닌다. 그래핀을 합성하거나 얻는 방법에는, 기계적 박리법(Micro mechanical exfoliation), 산화흑연(graphite oxide)을 이용한 reduced graphene oxide(RGO)방법과 탄화 규소(SiC)를 이용한 epitaxial growth 방법 등이 있지만, 대 면적화가 어렵거나 구조적 결함이 큰 문제점이 있다. 반면, 탄화수소(hydrocarbon)를 탄소 공급원으로 하는 열화학 기상 증착법(Thermal chemical vapor deposition, TCVD)은 구조적 결함이 상대적으로 적으면서 대 면적화가 가능하다는 이점 때문에 최근 가장 많이 이용되고 있는 방법이다. TCVD를 이용, 니켈, 몰리브덴, 금, 코발트 등의 금속에서 그래핀 합성연구가 보고되었지만, 대부분 수 층(fewlayer)의 그래핀이 합성되었다. 하지만, 구리 촉매를 이용하는 것이 단층 그래핀 합성에 매우 효율적이라는 연구결과가 보고되었다. 구리의 경우, 낮은 탄소융해도(solubility of carbon) 때문에 표면에서 self limiting 과정을 통하여 단층 그래핀이 합성된다. 그러나 단층 그래핀 일지라도 면저항(sheet resistance)이 매우 높고, 이론적 계산값에 비해 전자이동도(electron mobility)가 낮게 측정된다. 이러한 원인은 구조적 결함에서 기인된 것으로써 산업으로의 응용을 어렵게 만들기 때문에 양질의 단층 그래핀 합성연구는 필수적이다[1,2]. 본 연구에서는 TCVD를 이용하여 구리 포일(25 ${\mu}m$, Alfa Aeser) 위에 메탄가스를 탄소공급원으로 하여 수소를 함께 주입하고, 메탄가스의 양과 합성시간, 열처리 시간을 조절하면서 균일한 단층 그래핀을 합성하였다. 합성된 그래핀을 $SiO_2$ (300 nm)기판위에 전사(transfer)후 라만 분광법(raman spectroscopy)과 광학 현미경(optical microscope)을 통하여 분석하였다. 그 결과, 열처리 시간이 증가할수록 촉매로 사용된 구리 포일의 grain size가 커짐을 확인하였으며, 구리 포일 위에 합성된 그래핀의 grain size는, 구리 포일의 grain size에 의존하여 커짐을 확인하였다. 또한 동일한 grain 내의 그래핀은 균일한 층으로 합성되었다. 이는 기계적 박리법, RGO 방법, epitaxial growth 방법으로 얻은 그래핀과 비교하여 매우 뛰어난 결정성을 지님이 확인되었다. 본 연구를 통하여 면적이 넓으면서도 결정성이 매우 뛰어난 양질의 단층 그래핀 합성 방법을 확립하였다.

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Effect of Low Temperature Heat Treatment on the Physical and Chemical Properties of Carbon Anode Materials and the Performance of Secondary Batteries (저온 열처리가 탄소 음극재의 물리·화학적 특성 및 이차전지 성능에 미치는 영향)

  • Whang, Tae Kyung;Kim, Ji Hong;Im, Ji Sun;Kang, Seok Chang
    • Applied Chemistry for Engineering
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    • v.32 no.1
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    • pp.83-90
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    • 2021
  • In this study, effects of the physical and chemical properties of low temperature heated carbon on electrochemical behavior as a secondary battery anode material were investigated. A heat treatment at 600 ℃ was performed for coking of petroleum based pitch, and the manufactured coke was heat treated with different heat temperatures at 700~1,500 ℃ to prepare low temperature heated anode materials. The physical and chemical properties of carbon anode materials were studied through nitrogen adsorption and desorption, X-ray diffraction (XRD), Raman spectroscopy, elemental analysis. Also the anode properties of low temperature heated carbon were considered through electrochemical properties such as capacity, initial Coulomb efficiency (ICE), rate capability, and cycle performance. The crystal structure of low temperature (≤ 1500 ℃) heated carbon was improved by increasing the crystal size and true density, while the specific surface area decreased. Electrochemical properties of the anode material were changed with respect to the physical and chemical properties of low temperature heated carbon. The capacity and cycle performance were most affected by H/C atomic ratio. Also, the ICE was influenced by the specific surface area, whereas the rate performance was most affected by true density.

Characterization of Materials and Color Formation for Black Potteries from the Proto-Three Kingdoms Period in Ulsan, Korea (울산지역 원삼국시대 흑색토기의 재질 및 발색 특성)

  • Kim, Su Kyoung;Jang, Sungyoon;Lee, Chan Hee
    • Journal of Conservation Science
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    • v.37 no.2
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    • pp.77-89
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    • 2021
  • In this study, materials and color formation techniques were assessed for black potteries excavated from the Janghyeon-dong, Jungsan-dong and Gyodong-ri sites during the Proto-Three Kingdoms period in Ulsan, Korea. Although the black potteries were black superficially, the inner cores were either black or reddish yellow. Microscopy analysis identified that body clay was used for reddish iron oxide rich soils with quartz, alkali feldspar and mica, along with grains of myrmechite texture. Additionally, as marginal differences exist in the contents of SiO2, Fe2O3 and CaO, the composition of the host rock and clay distributed around the sites was affected. Thus, we can deduce that pottery was made by soiling at a short distance. Raman spectroscopy results revealed that the black layer of the black pottery was used as amorphous combustion carbon. In addition, as a transparent layer of brown lacquer was observed on the substrate that was in contact with the surface layer, the black layer of the pottery induced black color development by a combination of combustion carbon and lacquer. Based on the mineral composition and microtexture of the body clay, the firing temperature of the potteries seemed to range from 750 to 850℃, whereas the lacquer layer was pyrolyzed at 468℃ by thermal analysis. Therefore, a combined layer of combustion carbon and lacquer, which formed the black color, was painted after the body clay was fired.

Electrochemical Properties of SiOx Anode for Lithium-Ion Batteries According to Particle Size and Carbon Coating (입자 크기 및 탄소 코팅에 따른 리튬이온배터리용 SiOx 음극활물질의 전기화학적 특성)

  • Anna Park;Byung-Ki Na
    • Korean Chemical Engineering Research
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    • v.62 no.1
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    • pp.19-26
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    • 2024
  • In this study, the electrochemical properties of SiOx@C composite materials were prepared to alleviate volume expansion and cycle stability of silicon and to increase the capacity of anode material for LIBs. SiO2 particles of 100, 200, and 500 nm were synthesized by the Stӧber method, and reduced to SiOx (0≤x≤2) through the magnesiothermic reduction method. Then, SiOx@C anode materials were synthesized by carbonization of PVC on SiOx. The physical properties of prepared SiOx and SiOx@C anode materials were analyzed by XRD, SEM, TGA, Raman spectroscopy, XPS and BET. The electrochemical properties were investigated by cycling performance, rate performance, CV and EIS test. As a result, the SiOx@C-7030 manufactured by coating carbon at SiOx : C = 70 : 30 on a 100 nm SiOx with the smallest particle size showed the best electrochemical properties with a discharge capacity of 1055 mAh/g and a capacity retention rate of 81.9% at 100 cycles. It was confirmed that cycle stability was impoved by reducing particle size and carbon coating.