• Title/Summary/Keyword: Spectroscopy

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Comparative Study on The Composition of Essential Oil by Supercritical Carbon Dioxide Extraction and Hydro-distillation from Chamaecyparis obtusa Leaves (편백 잎에서 추출한 정유와 초임계 이산화탄소 추출물의 성분 비교분석)

  • Kim, Jae-Woo;Choi, Won-Sil;Lee, Sung-Suk;Park, Mi-Jin
    • Journal of the Korean Wood Science and Technology
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    • v.43 no.4
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    • pp.494-503
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    • 2015
  • This study was focused on the comparison of the variations in the yield and chemical composition of Chamaecyparis obtusa leaf oil obtained under different pressure conditions of the supercritical carbon dioxide extraction (SCE), and by hydro-distillation. SCE was carried out varying the pressure in the range of 100~400 bar at $40^{\circ}C$. The chemical composition of C. obtusa leaf oils was determined by gas chromatography-mass spectroscopy (GC-MS) analysis. The maximum yield of 4.4% (relative to the initial mass of oven dry mass) was obtained in the extraction under 300 bar pressure, which was higher than that of the hydro-distillation method (1.9%). The contents of sesquiterpenes in the extracts obtained by the SCE were higher than those of the essential oils of C. obtusa by the hydro-distillation. The sesquiterpenes in the SCE extracts made up approximately 39%~46% of the total, followed by monoterpenes, diterpene, and lignan. The contents of each constituent in the supercritical carbon dioxide extracts were varied on the extraction pressure. Therefore, these results showed that the extraction condition of SCE had significant effect on the yield of C. obtusa oils and its chemical composition.

Synthesis of High-Quality Single-Walled Carbon Nanotube Fibers by Vertical CVD (수직 가열로를 이용한 고순도 단일벽 탄소나노튜브 섬유의 합성)

  • Kim, Tae-Min;Song, Woo-Seok;Kim, Yoo-Seok;Kim, Soo-Youn;Choi, Won-Chel;Park, Chong-Yun
    • Journal of the Korean Vacuum Society
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    • v.19 no.5
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    • pp.377-384
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    • 2010
  • Many routes have been developed for the synthesis of signle-walled carbon nanotubes (SWCNTs). We spun fibers of SWCNTs directly from vertical furnace using a liquid source of carbon and an iron-contained molecule. The solution was prepared by ethanol as a carbon source, in which ferrocene as a catalyst, thiophene were dissolved. It was then injected from the top of the furnace into hot zone with hydrogen as a carrier gas. We successfully synthesized high-quality SWCNTs by adjusting the various experimental conditions, such as concentration of ferrocene, solution injection rate, concentration of thiophene, and hydrogen flow rate. Measurement of Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy were carried out to find the optimized conditions. The synthesized SWCNTs (1.16~1.64 nm) appeared a bundle structure and well-aligned parallel to the direction of furnace. These results also provide an simple way for high-quality SWCNTs mass production and fabricating direct spining SWCNTs fiber. It will allow one-step production of SWCNTs fiber with potentially excellent properties and wide-range applications.

Preparation and Characterization of Random Copolymer Electrolyte Membranes Containing PFCB (Perfluorocyclobutane) Group (PFCB (Perfluorocyclobutane) Group을 포함한 랜덤 공중합체 고분자 전해질 막 제조 및 특성연구)

  • Kim Jeong-Hoon;Kim Dong-Jin;Chang Bong-Jun;Lee Soo-Bok;Joo Hyeok-Jong
    • Membrane Journal
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    • v.16 no.3
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    • pp.221-229
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    • 2006
  • This study is about the preparation and characterization of sulfonated random copolymer membranes containing perfluorocyclobutane (PFCB), fluorenyl, and sulfonyl units. The polymers were prepared through three synthetic steps, that is, the synthesis of a trofluorovinylether-terminated monomer, its thermal polymerization, and post-sulfonation using chlorosulfonic acid. A series of sulfonated random copolymers with different ion exchange capacity (IEC) were prepared by changing contents of fluorenyl uints in polymers with fixed molar ratio of chlorosulfonic acid during the post-sulfonation reaction. All the synthesized compounds were characterized by FT-lR, $^1H-NMR$, $^{19}F-NMR$, and Mass spectroscopy. As the content of sulfonated fluorenyl units increased, the IEC, water uptake, and ion conductivity of the sulfonated random copolymer membranes increased. The sulfonated random copolymer S-1 and S-2 showed higher values of ion conductivity than the Nafion-115 in a wide range of temperatures ($25{\sim}80^{\circ}C$).

Assessment of Emitted Volatile Organic Compounds, Metals and Characteristic of Particle in Commercial 3D Printing Service Workplace (실제 3D 프린팅 작업장에서 발생하는 공기 중 유기화합물, 금속 및 입자특성 평가)

  • Kim, Sungho;Chung, Eunkyo;Kim, Seodong;Kwon, Jiwoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.30 no.2
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    • pp.153-162
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    • 2020
  • Objectives: 3D printing technologies have become widely developed and are increasingly being used for a variety of purposes. Recently, the evaluation of 3D printing operations has been conducted through chamber test studies, and actual workplace studies have yet to be completed. Therefore, the objective of this study was to determine the emission of volatile organic compounds(VOCs), metals, and particles from printing operations at a workplace. This included monitoring conducted at a commercial 3D printing service workplace where the processes involved material extrusion, material jetting, binder jetting, vat photo polymerization, and powder bed fusion. Methods: Area samples were collected with using a Tenax TA tube for VOC emission and MCE filter for metals in the workplace. For particle monitoring, Mini Particle Samplers(MPS) were also placed in the printer, indoor work area, and outdoor area. The objective was to analyze and identify particles' size, morphology, and chemical composition using transmission electron microscopy with energy dispersive spectroscopy(TEM-EDS) in the workplace. Results: The monitoring revealed that the concentration of VOCs and metals generated during the 3D printing process was low. However, it also revealed that within the 3D printing area, the highest concentration of total volatile organic compounds(TVOC) was 4,164 ppb at the vat photopolymerization 3D printing workplace, and the lowest was 148 ppb at the material extrusion 3D printing workplace. For the metals monitoring, chromium, which, is carcinogenic for humans, was detected in the workplace. As a characteristic of the particles, nano-sized particles were also found during the monitoring, but most of them were agglomerated with large and small particles. Conclusions: Based on the monitoring conducted at the commercial 3D printing operation, the results revealed that the concentration of VOCs and metals in the workplace were within Korea's occupational exposure limits. However, due to the emission of nano-sized particles during 3D printing operations, it was recommended that the exposure to VOCs and metals in the workplace should be minimized out of concern for workers' health. It was also shown that the characteristics of particles emitted from 3D printing operations may spread widely within an indoor workplace.

Detoxification of Glutaraldehyde Treated Porcine Pericardium Using L-arginine & $NABH_4$

  • Kim, Kwan-Chang;Kim, Soo-Hwan;Kim, Yong-Jin
    • Journal of Chest Surgery
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    • v.44 no.2
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    • pp.99-107
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    • 2011
  • Background: Calcification is the most frequent cause of clinical failure of bioprosthetic tissues fabricated from GA-fixed porcine valves or bovine pericardium. A multi-factorial approach using different mechanisms was recently developed to reduce the calcification of bioprosthetic tissues. The purpose of the present study was to evaluate the synchronized synergism of using L-arginine and $NaBH_4$, compared with ethanol and L-lysine, in glutaraldehyde treated porcine pericardium from the standpoint of calcification and tissue elasticity. Materials and Methods: Porcine pericardium was fixed at 0.625% GA (7 days at room temperature after 2 days at $4^{\circ}C$). An interim step of ethanol (80%; 1 day at room temperature) or L-lysine (0.1 M; 2 days at $37^{\circ}C$) or L-arginine (0.1 M; 2 days at $37^{\circ}C$) was followed by completion of the GA fixation. A final step of NaBH4 (0.1 M; 2 days at room temperature) was followed. Their tensile strength, thickness, and thermal stability were measured. Treated pericardia were implanted subcutaneously into three-week-old Sprague-Dawley rats for 8 weeks. Calcium content was assessed by atomic absorption spectroscopy and histology. Results: L-arginine and $NaBH_4$ pretreatment ($1.81{\pm}0.39$ kgf/5 mm p=0.001, $0.30{\pm}0.08$ mm p<0.001) significantly increased tensile strength and thickness compared with the control ($0.53{\pm}0.34$ kgf/5 mm, $0.10{\pm}0.02$ mm). In a thermal stability test, L-arginine and $NaBH_4$ pretreatment ($84.25{\pm}1.12^{\circ}C$, p=0.023) caused a significant difference from the control ($86.25{\pm}0.00^{\circ}C$). L-lysine and $NaBH_4$ pretreatment ($183.8{\pm}42.6$ ug/mg, p=0.804), and L-arginine and $NaBH_4$ pretreatment ($163.3{\pm}27.5$ ug/mg, p=0.621) did not significantly inhibit calcification compared to the control ($175.5{\pm}45.3$ ug/mg), but ethanol and $NaBH_4$ pretreatment did ($38.5{\pm}37.3$ ug/mg, p=0.003). Conclusion: The combined pretreatment using L-arginine and $NaBH_4$ after GA fixation seemed to increase the tensile strength and thickness of porcine pericardium, fixed with GA. Additionally, it seemed to keep thermal stability. However it could not decrease the calcification of porcine pericardium fixed with GA. $NaBH_4$ pretreatment seemed to decrease the calcification of porcine pericardium fixed with GA, but only with ethanol.

Control of Graphene's Electrical Properties by Chemical Doping Methods

  • Lee, Seung-Hwan;Choi, Min-Sup;La, Chang-Ho;Yoo, Won-Jong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.119-119
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    • 2011
  • This study examined the synthesis of large area graphene and the change of its characteristics depending on the ratio of CH4/H2 by using the thermal CVD methods and performed the experiments to control the electron-hole conduction and Dirac-point of graphene by using chemical doping methods. Firstly, with regard to the characteristics of the large area graphene depending on the ratio of CH4/H2, hydrophobic characteristics of the graphene changed to hydrophilic characteristics as the ratio of CH4/H2 reduces. The angle of contact also increased to 78$^{\circ}$ from 58$^{\circ}$. According to the results of Raman spectroscopy showing the degree of defect, the ratio of I(D)/I(G) increases to 0.42% from 0.25% and the surface resistance also increased to 950 ${\Omega}$ from 750 ${\Omega}$/sq. As for the graphene synthesis at the high temperature of 1,000$^{\circ}$ by using CH4/H2 in a Cu-Foil, the possibility of graphene formation was determined as a function of the ratio of H2 included in the fixed quantity of CH4 as per specifications of every equipment. It was observed that the excessive amount of H2 prevented graphene from forming, as extra H-atoms and molecules activated the reaction to C-bond of graphene. Secondly, in the experiment for the electron-hole conduction and the Dirac-point of graphene using the chemical doping method, the shift of Dirac-point and the change in the electron-hole conduction were observed for both the N-type (PEI) and the P-type (Diazonium) dopings. The ID-VG results show that, for the N-type (PEI) doped graphene, Dirac-point shifted to the left (-voltage direction) by 90V at an hour and by 130 V at 2 hours respectively, compared to the pristine graphene. Carrier mobility was also reduced by 1,600 cm2/Vs (1 hour) and 1,100 cm2/Vs (2 hours), compared to the maximum hole mobility of the pristine graphene.

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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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InAs/GaAs 양자점 태양전지에서 AlGaAs Potential Barrier 두께에 따른 Photoreflectance 특성 및 내부 전기장 변화

  • Son, Chang-Won;Ha, Jae-Du;Han, Im-Sik;Kim, Jong-Su;Lee, Sang-Jo;Smith, Ryan;Kim, Yeong-Ho;Kim, Seong-Jun;Lee, Sang-Jun;No, Sam-Gyu;Park, Dong-U;Kim, Jin-Su;Im, Jae-Yeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.306-307
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    • 2011
  • Franz Keldysh Oscillation (FKO)은 p-n 접합 구조의 공핍층(depletion zone)에서 전기장(electric field)에 의해 발생되며, Photoreflectance (PR) spectroscopy를 통하여 관측된다. InAs/GaAs 양자점 태양전지(Quantum Dot Solar Cells, QDSCs)에서 PR 신호에 대한 Fast Fourier Transform (FFT)을 통하여 FKO 주파수들을 관측할 수 있고, 각각의 FKO 주파수들은 태양전지 구조에 대응하는 표면 및 내부전기장(internal electric field) 들로 분류할 수 있다. InAs/GaAs 양자점 태양전지에서 AlGaAs potential barrier의 두께에 따른 내부전기장의 변화를 조사하기 위해, GaAs-matrix에 8주기의 InAs 양자점 층이 삽입된 태양전지를 molecular beam epitaxy (MBE) 방법으로 성장하였다. 양자점의 크기는 2.0 monolayer (ML)이며, 각 양자점 층은 1.6 nm에서 6.0 nm의 AlGaAs potential barrier들로 분리되어 있다. 또한 양자점 층의 위치에 따라 내부전기장 변화를 조사하기 위해, p-i-n 구조에서 양자점 층이 공핍층 내에 위치한 경우와 p+-n-n+ 구조에서 양자점 층이 공핍 층으로부터 멀리 떨어진 n-base 영역에 삽입하여 실험결과를 비교분석하였다. PR 실험결과로부터, p-i-n 구조에서 InAs 양자점 태양전지의 내부전기장 변화는 potential barrier 두께에 따라 다소 복잡한 변화를 보였으며, 이는 양자점 층이 공핍층 내에 위치함으로써 격자 불일치(lattice mismatch)로 발생된 응력(strain)의 영향으로 설명할 수 있다. 이러한 결과들을 각각의 태양전지 구조에서 표면 및 내부전기장에 대해 계산된 값들에 근거하여, p+-n-n+ 구조에서 양자점 층이 공핍 층으로부터 멀리 떨어진 영역에 삽입된 경우의 결과와 비교해 보면 내부전기장의 변화는 더욱 분명해진다. 즉, 양자점 층의 potential barrier의 두께를 조절하거나, 양자점 층의 위치를 변화시킴으로써 양자점 태양전지의 내부전기장을 조작할 수 있으며, 이는 PR 실험을 통해 FKO를 관측함으로써 확인할 수 있다.

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Hydrothermal Synthesis and Structural Characterization of x mol% Calcia-Stabilized ZrO2 Nanopowders (x mol% 칼시아-안정화 지르코니아 나노분말의 수열합성 및 구조적 특성평가)

  • Ryu, Je-Hyeok;Moon, Jung-In;Park, Yeon-Kyung;Nguyen, Tuan Dung;Song, Jeong-Hwan;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.220-226
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    • 2012
  • Pure zirconia and $x$ mol% calcia partially stabilized zirconia ($x$ = 1.5, 3, and 8) nanopowders were synthesized by hydrothermal method with various reaction temperatures for 24 hrs. The precipitated precursor of pure zirconia and $x$ mol% calcia doped zirconia was prepared by adding $NH_4OH$ to starting solutions; resulting sample was then put into an autoclave reactor. The optimal experimental conditions, such as reaction temperatures and times and amounts of stabilizer CaO, were carefully studied. The synthesized $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5, 3, and 8) powders were characterized by XRD, SEM, TG-DTA, and Raman spectroscopy. When the hydrothermal temperature was as low as $160^{\circ}C$, pure $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5 and 3) powders were identified as a mixture of monoclinic and tetragonal phases. However, a stable tetragonal phase of zirconia was observed in the 8 mol% calcia doped zirconia nanopowder at hydrothermal temperature above $160^{\circ}C$. To observe the phase transition, the 3 mol% CaO-$ZrO_2$ and 8 mol% CaO-$ZrO_2$ nanopowders were heat treated from 600 to $1000^{\circ}C$ for 2h. The 3 mol% CaO-$ZrO_2$ heat treated at above $1000^{\circ}C$ was found to undergo a complete phase transition from mixture phase to monoclinic phase. However, the 8 mol% calcia doped zirconia appeared in the stable tetragonal phase after heat treatment. The result of this study therefore should be considered as the preparation of 8 mol% CaO-$ZrO_2$ nanopowders via the hydrothermal method.

Fundamental Studies on the Development of On-line Monitoring of Trace Mercury in Drinking Water (음용수 중 수은 연속자동측정시스템의 개발에 관한 연구)

  • Chang, Soo-Hyun;Kim, Hyo-Jin;Kim, Sun-Tae;Kim, Young-Man
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.299-305
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    • 1999
  • The electrolyte cathode atomic glow discharge (ELCAD) is a new plasma source for direct determination of trace heavy metals in drinking and waste water. ELCAD has been successfully developed for on-line monitoring of heavy metals, however, shows difficulty to measure mercury. In this study, ELCAD has been modified to apply the atomic absorption spectrometry (AAS) for the direct determination of trace elements of mercury in flowing water.The fundamental characteristics of this new types of plasma source have been investigated and found that the pH of the solution, discharge voltage, and current are most important factors.The absorbance of 1.0 ppm Hg standard solution increases as pH of the solution increases from pH 1.0 to 3.0.However, % RSD of the absorbance also increases as the pH of solution increasesdue to plasma unstability.The detection limits of the standard solution of pH 1.5 and pH 3.0 are about 40 ppb and 10 ppb level, respectively.

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