• Title/Summary/Keyword: 전자 분광 화학분석법

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A Study on Oxygen Evolution Activity of Co3O4 with different morphology prepared by Ultrasonic Spray Pyrolysis for Water Electrolysis (분무열분해로 합성한 수전해용 Co3O4의 입자형태에 따른 산소발생 활성에 관한 연구)

  • Kim, Ingyeom;Nah, In Wook;Park, Sehkyu
    • Korean Chemical Engineering Research
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    • v.54 no.6
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    • pp.854-862
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    • 2016
  • As the demand for a clean energy to replace fossil fuel being depleted increases, hydrogen energy is considered as a promising candidate for future energy source. Water electrolysis which produces hydrogen has high energy efficiency and stability but still has a large overpotential for oxygen evolution reaction (OER). In this study, $Co_3O_4$ catalysts with different morphology were prepared by spray pyrolysis from solutions which contain Co precursor and various organic additives (urea, sucrose, and citric acid), followed by post heat treatment. For the catalysts synthesized, X-ray diffraction (XRD) measurements were performed to identify their crystal structure. Morphology and surface shape of the catalysts were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Surface area and pore volume were examined by nitrogen adsortpion & desorption tests and X-ray photoelectron spectroscopy (XPS) was conducted to confirm nitrogen doping. Linear sweep voltammetry (LSV) was carried out to investigate OER activity of $Co_3O_4$ catalysts. As a result, bare-$Co_3O_4$ which has high surface area and small particle size determined by spray pyrolysis showed high activity toward OER.

Mineralogy and Genesis of the Sungsan Clay Deposits (聲山납석광상의 광물학적 및 성인적 연구)

  • Cho, Hyen-Goo;Kim, Soo-Jin
    • Journal of the Mineralogical Society of Korea
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    • v.7 no.1
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    • pp.14-24
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    • 1994
  • The Sungsan clay deposits have been formed by the hydrothermal alteration of volcanic and volcanoclastic rocks of the Hwangsan Formation of Cretaceous age. Claystones are mainly composed of dickite, alunite, illitic minerals and tosudite. The mineralogical properties of clay minerals have been studied using X-ray diffraction analysis, electron microscopy, electron microprobe analysis, and infrared absorption analysis. The physicochemical condition for the clay deposits also have been studied by the activity diagrams and mineral assemblages. Dickite, the dominant mineral in clay deposits, occurs generally as massive aggregates. It shows book-structure of well-defined hexagonal plates. Chemistry of dickite agrees with its ideal formula. Peak depth ratios in infrared absorption spectra were used for discrimination between pure and mixture of kaolin minerals. Five hydrothermal alteration zones are divided according to the mineral assemblages. From center to margin, alunite, dickite, illite and albite zones are discernible. Quartz zone occurs as small lenticular form in dickite zone. The formation of dickite and illite zones are promoted by decreasing $a_{k^+}$. An increase in $a_{H_{2}SO_{4}}$ or $a_{K_{2}SO_{4}}$ is required for the formation of alunite zone. Estimated temperature of formation ranges 110-270 $^{\circ}C$

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Dye-Sensitized Solar Cell Based on TiO2-Graphene Composite Electrodes (TiO2와 Graphene 혼합물을 전극으로 사용한 염료감응형 태양전지특성 연구)

  • Battumur, T.;Yang, Wooseung;Ambade, S.B.;Lee, Soo-Hyoung
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.177-181
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    • 2012
  • Dye-sensitized solar cells(DSSCs) based on $TiO_2$ film photo anode incorporated with different amount of grapheme nanosheet(GNS) are fabricated and their photovoltaic performance are investigated. The $TiO_2$-GNS composite electrode has been prepared by a direct mixing method. The DSSC performance of this composite electrode was measured using N3 dye as a sensitizer. The performance of DSSCs using the $TiO_2$-GNS composite electrodes is dependent on the GNS loading in the electrodes. The results show that the DSSCs incorporating 0.01 wt% GNS in $TiO_2$photo anode demonstrates a maximum power conversion efficiency of 5.73%, 26% higher than that without GNS. The performance improvement is ascribed to increased N3 dye adsorption, the reduction of electron recombination and back transport reaction as well as enhancement of electron transport with the introduction of GNS. The presence of both $TiO_2$(anatase) and GNS has been confirmed by FieldEmission Scanning Electron Microscopy(FE-SEM). The decrease in recombination due to GNS in DSSCs has been investigated by the Electrochemical Impedance Spectroscopy.

Physicochemical Property and Release Behavior of Ibuprofen Solid Dispersion with Cellulose Acetate Prepared with Various Methods (이부프로펜과 셀룰로오스아세테이트의 고체분산체 제조방법에 따른 물리화학적 성질 및 용출 특성)

  • Lee, Eun-Yong;Oh, Myeong-Jun;Kim, Se-Ho;Seong, Kyong-Yeol;Lee, Young-Hyun;Kim, Soo-Jin;She, Han-Sol;Lee, Dong-Won;Khang, Gil-Son
    • Polymer(Korea)
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    • v.35 no.2
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    • pp.113-118
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    • 2011
  • Solid dispersion is used to improve the solubility of water-insoluble drug. Release properties depend on the characteristics of polymer and the physicochemical properties of solid dispersion. In this study the solid dispersions of ibuprofen and cellulose acetate were prepared using spray-drying and rotary evaporation. The physicochemical properties of the solid dispersions were analyzed by SEM, XRD, DSC, and FTIR. The hydrophilicity of polymer was analyzed by measuring the contact angle of water. The results of DSC and XRD analysis demonstrated that the crystallinity of ibuprofen was changed by solid dispersion preparation. The results of contact angle showed that hydrophilicity was proportional to polymer content. Release profile showed that for solid dispersion. the release rate of ibuprofen decreased as polymer content increased in intestinal juice (pH 6.8). The dissolution rate of ibuprofen was improved with increasing polymer content in gastric juice (pH 1.2).

Effect of pyrolysis temperature and pressing load on the densification of amorphous silicon carbide block (열분해 온도와 성형압력의 영향에 따른 비정질 탄화규소 블록의 치밀화)

  • Joo, Young Jun;Joo, Sang Hyun;Cho, Kwang Youn
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.6
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    • pp.271-276
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    • 2020
  • In this study, an amorphous SiC block was manufactured using polycarbosilane (PCS), an organosilicon polymer. The dense SiC blocks were easily fabricated in various shapes via pyrolysis at 1100℃, 1200℃, 1300℃, 1400℃ after manufacturing a PCS molded body using cured PCS powder. Physical and chemical properties were analyzed using a thermogravimetric analyzer (TGA), scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and universal testing machine (UTM). The prepared SiC block was decomposed into SiO and CO gas as the temperature increased, and β-SiC crystal grains were grown in an amorphous structure. In addition, the density and flexural strength were the highest at 1.9038 g/㎤ and 6.189 MPa of SiC prepared at 1100℃. The manufactured amorphous silicon carbide block is expected to be applicable to other fields, such as the previously reported microwave assisted heating element.

Methylene Blue Photodegradation Properties of Anatase/brookite Hybrid TiO2 Photocatalyst Prepared with Different Acid Catalysts (산 촉매에 따른 아나타제/브루카이트 혼성형 TiO2 광촉매의 메틸렌블루 광분해특성)

  • Yun, Seok-Min;Kim, Jinhoon;Jeong, Euigyung;Im, Ji Sun;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.22 no.1
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    • pp.21-25
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    • 2011
  • In this study, anatase/brookite hybrid $TiO_2$ was prepared using different acid catalysts and microwave to improve photodegradation of organic pollutants. The methylene blue photodegradation properties of the prepared photocatalysts with different particle/crystal size and brookite fractions were investigated. Surface characteristics and particle sizes of anatase/brookite hybrid $TiO_2$ were evaluated using scanning electron microscopy (SEM) and laser diffraction particle size analyzer, respectively and crystal structures were investigated with X-ray diffraction (XRD). Methylene blue photodegradation properties were evaluated with UV-vis spectrophotometer. Anatase and anatase/brookite hybrid $TiO_2$ had less than 500 nm size of clusters and the average particle size of $6.66{\sim}6.85{\mu}m$, suggesting that types of acid catalysts did not affect the size. XRD of the prepared $TiO_2$ showed that the photocatalysts had anatase/brookite hybrid crystal structure and applying microwave did not change their crystal structure. Photodegradation of methylene blue with the prepared photocatalyst did not increased proportionally to the fraction of brookite and the crystal size and decreased when brookite fraction and the crystal size increased further. Anatase/brookite hybrid $TiO_2$ with brookite fraction of 9.4% and crystal size of 4.53 nm shows the best photodegradation activity of methylene blue.

Effects of Increase in Ratio of Phenolic Hydroxyl Function on Carbon Fiber Surfaces by Anodic Oxidation on Mechanical Interfacial Bonding of Carbon Fibers-reinforced Epoxy Matrix Composites (양극산화 처리에 따른 탄소섬유 표면의 페놀릭 하이드록실 관능기 비율의 증가가 에폭시기지 복합재료의 기계적 계면결합 특성에 미치는 영향)

  • Kim, Dong-Kyu;Kim, Kwan-Woo;Han, Woong;Song, Bhumkeun;Oh, Sang-Yub;Bang, Yun Hyuk;Kim, Byung-Joo
    • Applied Chemistry for Engineering
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    • v.27 no.5
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    • pp.472-477
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    • 2016
  • We studied the effects of anodic oxidation treatments of carbon fibers on interfacial adhesion of the carbon fibers-reinforced epoxy matrix composites with various current densities. The surface of treated carbon fibers was characterized by atomic force microscope (AFM), field emission-scanning electron microscope (FE-SEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). The interlaminar shear strength (ILSS) of the composites was determined by a short beam shear test. This result showed that both the roughness and oxygen group of the carbon fibers surface increased in proportion to the current density. After anodic-oxidation-treated, the ILSS also increased as a function of the current density. In addition, the proportional relationship between ILSS and phenolic hydroxyl group was confirmed. The ILSS of the CF-2.0 sample increased by 4% compared to that of the CF-AS sample, because the anodic oxidation treatment increased the oxygen group and roughness on the carbon fibers surface, which leading to the improvement of the interfacial adhesion of the carbon fibers-reinforced epoxy matrix composites. Among these, the phenolic hydroxyl group which has the proportional relationship with ILSS is found to be the most important factor for improving the interfacial adhesion of the carbon fibers-reinforced epoxy matrix composites.

Chemical Age Dating of Zircon and Monazite by E1ectron Microprobe (전자현미분석기를 이용한 저어콘 및 모나자이트의 화학적 연대 측정법)

  • 이석훈
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.179-189
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    • 2001
  • The determination of trace concentration of U, Th and Pb was carried out for chemical dating of zircon and monazite by electron microprobe. Detection limit and error range should be considered to measure characteristic X-rays of M-line from those minerals, which are low in the ionization of atom and low peak intensity in the spectrum. The element of U, Th and Pb were simultaneously measured with 3 spectrometers equipped with PET crystal to reduce a total counting time and error due to drift of instrumental operating condition. Detection limit could be improved from increase of the peak/background ratio through adjusting pulse height analyzer about 1000 mv baseline. Under permissible maximum analytical conditions, theoretical detection limit of U, Th and Pb is down to 30 ppm (99% confidence level). The analytical result was maintained at a relative error $\pm$10% ($2{\sigma}$) in 800 ppm Pb, $\pm$5% ($2{\sigma}$) in 2330 ppm U and $\pm$10% ($2{\sigma}$) in dating from a single measurement of zircon at 15 keV and 100 nA. However, for the precise dating of zircon and monazite, if it is considered a 3 $\mu\textrm{m}$ spatial resolution, <100 ppm ($3{\sigma}$) detection limit and <$\pm$10% ($2{\sigma}$) relative error, optimum analytical conditions are given as 15~20 keV accelerating voltage, 100~200 nA beam current and 300~1200 sec total counting time. To reduce material damage by high current, there is need to be up to 3~5 $\mu\textrm{m}$ of electron beam diameter, or to use arithmetic average of multiple measuring at a shorter counting time. A younger or relatively low concentration rocks can be dated chemically by lower detection limit and improved precision resulted from increase of current and measuring time.

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Direct Conversion of Cellulose into Polyols over Pt Catalysts Supported on Zeolites (제올라이트에 담지된 백금 촉매를 이용한 셀룰로우스의 폴리올로의 직접 전환)

  • You, Su Jin;Baek, In Gu;Park, Eun Duck
    • Korean Chemical Engineering Research
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    • v.50 no.3
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    • pp.435-441
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    • 2012
  • The direct conversion of cellulose into polyols in $H_2$ was examined over Pt catalysts supported on various zeolites, viz., mordenite, Y, ferrierite, and ${\beta}$. For comparison, Pt catalysts supported on ${\gamma}-Al_2O_3$, $SiO_2-Al_2O_3$, and $SiO_2$ were also tested. The physical properties of the catalysts were probed with $N_2$ physisorption. The surface acidity was measured with temperature programmed desorption of ammonia ($NH_3$-TPD). The Pt content was quantified with inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The Pt dispersion was determined with CO chemisorptions and transmission electron microscopy (TEM). The conversion of cellulose appeared to be mainly dependent on the reaction temperature and reaction time because it depends on the concentration of $H^+$ ions reversibly formed in hot water. Pt/H-mordenite (20) showed the highest yield to polyols among the tested catalysts. Pt/H-zeolite was superior to Pt/Na-zeolite for this reaction. The polyol yield was dependent on the surface acid density and the external surface area.

Characterization of InAs Quantum Dots in InGaAsP Quantum Well Grown by MOCVD for 1.55 ${\mu}m$

  • Choe, Jang-Hui;Han, Won-Seok;Song, Jeong-Ho;Lee, Dong-Han
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.134-135
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    • 2011
  • 양자점은 전자와 양공을 3차원으로 속박 시키므로 기존의 bulk나 양자우물보다 양자점을 이용한 레이저 다이오드의 경우 낮은 문턱 전류, 높은 미분이득 및 온도 안전성의 장점이 있을 거라 기대되고 있다. 그러나, 양자점은 낮은 areal coverage 때문에 높은 속박효율을 얻지 못하고 있다. 이러한 양자점의 문제점을 해결하기 위해 양자점을 양자우물 안에 성장시켜 운반자들의 포획을 향상시키는 방법들이 연구되고 있다. 양자우물 안에 양자점을 넣으면 양자우물이 운반자들의 포획을 증가 시키고, 열적 방출도 억제하여 온도 안정성이 향상 되는 것으로 알려져 있다. 광통신 대역의 1.3 ${\mu}m$ 경우, GaAs계를 이용하여 InAs 양자점을 strained InGaAs 박막을 우물층으로 한 dot-in-a-well 구조의 연구는 몇몇 보고된 바 있다. 그러나 InP계를 사용하는 1.55 ${\mu}m$ 대역에서 dot-in-a-well구조의 연구는 아직 미미하다. 본 연구에서는 유기 금속 화학 증착법(metal organic chemical vapor deposition)을 이용하여 InP 기판 위에 InAs 양자점을 자발성장법으로 성장하였으며 dot-in-a-well 구조에서 우물층으로 1.35 ${\mu}m$ 파장의 $In_{0.69}Ga_{0.31}As_{0.67}P_{0.33}$ (1.35Q)를, 장벽층으로는 1.1 ${\mu}m$ 파장의 $In_{0.85}Ga_{0.15}As_{0.32}P_{0.68}$(1.1Q)를 사용하였다. 양자우물층과 장벽층은 모두 InP 기판과 격자가 일치하는 조건으로 성장하였다. III족 원료로는 trimethylindium (TMI)와 trimethylgalium (TMGa)을 사용하였으며 V족 원료 가스로는 $PH_3$ 100%, $AsH_3$ 100%를, carrier gas로는 $H_2$를 사용하였다. InP buffer층의 성장 온도는 640$^{\circ}C$이며 양자점 성장 온도는 520$^{\circ}C$이다. 양자점 형성은 원자력간 현미경(Atomic force microscopy)를 이용하여 확인하였으며, 박막의 결정성은 쌍결정 회절분석(Double crystal x-ray deffractometry)를 이용하여 확인하였다. 확인된 성장 조건을 이용하여 양자점 시료를 성장하였으며 광여기분광법(Photoluminescence)을 이용하여 광특성을 분석하였다. Fig. 1은 dot in a barrier 와 dot-in-a-well 시료의 성장구조이다. Fig. 1(a)는 일반적인 dot-in-a-barrier 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장한 후 양자점을 성장하였다. 그 후 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 1(b)는 dot-in-a-well 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장 후 1.35Q 우물층을 4 nm 성장하였다. 그 위에 InAs 양자점을 성장하였다. 그 후에 1.35Q 우물층을 4 nm 성장하고 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 2는 dot-in-a-barrier 시료와 dot-in-a-well 시료의 상온 PL data이다. Dot-in-a-barrier 시료의 PL 파장은 1544 nm이며 반치폭은 79.70 meV이다. Dot-in-a-well 시료의 파장은 1546 nm이며 반치폭은 70.80 meV이다. 두 시료의 PL 파장 변화는 없으며, 반치폭은 dot-in-a-well 시료가 8.9 meV 감소하였다. Dot-in-a-well 시료의 PL peak 강도는 57% 증가하였으며 적분강도(integration intensity)는 45%가 증가하였다. PL 데이터에서 높은 에너지의 반치폭 변화는 없으며 낮은 에너지의 반치폭은 8 meV 감소하였다. 적분강도 증가에서 dot-in-a-well 구조가 dot-in-a-barrier 구조보다 전자-양공의 재결합이 증가한다는 것을 알 수 있으며, 반치폭 변화로부터 특히 높은 에너지를 갖는 작은 양자점에서의 재결합이 증가 된 것을 알 수 있다. 이는 양자우물이 장벽보다 전자-양공의 구속력을 증가시키기 때문에 양자점에 전자와 양공의 공급을 증가시키기 때문이다. 따라서 낮은 에너지를 가지는 양자점을 모두 채우고 높은 에너지를 가지는 양자점까지 채우게 되므로, 높은 에너지를 가지는 양자점에서의 전자-양공 재결합이 증가되었기 때문이다. 뿐만 아니라 파장 변화 없이 PL peak 강도와 적분강도가 증가하고 낮은 에너지 쪽의 반치폭이 감소한 것으로부터 에너지가 낮은 양자점보다는 에너지가 높은 양자점에서의 전자-양공 재결합율이 급증하였음을 알 수 있다. 우리는 이와 같은 연구에서 InP계를 이용해 1.55 ${\mu}m$에서도 dot in a well구조를 성장 하여 더 좋은 특성을 낼 수 있으며 앞으로 많은 연구가 필요할 것이라 생각한다.

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