• 제목/요약/키워드: in situ Raman Spectroscopy

검색결과 30건 처리시간 0.043초

Novel Composite Membranes Comprising Silver Salts Physically Dispersed in Poly(ethylene-co-propylene) for the Separation of Propylene/Propane

  • Kim, Jong-Hak;Min, Byoung-Ryul;Kim, Yong-Woo;Kang, Sang-Wook;Won, Jong-Ok;Kang, Yong-Soo
    • Macromolecular Research
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    • 제15권4호
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    • pp.343-347
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    • 2007
  • Novel composite membranes, which delivered high separation performance for propylene/propane mixtures, were developed by coating inert poly(ethylene-co-propylene) rubber (EPR) onto a porous polyester substrate, followed by the physical distribution of $AgBF_4$. Scanning electron microscopy-wavelength dispersive spectrometer (SEM-WDS) revealed that silver salts were uniformly distributed in the EPR layer. The physical dispersion of the silver salts in the inert polymer matrix, without specific interaction, was characterized by FT-IR and FT-Raman spectroscopy. The high separation performance was presumed to stem from the in-situ dissolution of crystalline silver ionic aggregates into free silver ions, which acted as an active propylene carrier within a propylene environment, leading to facilitated propylene transport through the membranes. The membranes were functional at all silver loading levels, exhibiting an unusually low threshold carrier concentration (less than 0.06 of silver weight fraction). The separation properties of these membranes, i.e. the mixed gas selectivity of propylene/propane ${\sim}55$ and mixed gas permeance ${\sim}7$ GPU, were stable for several days.

토양, 지하수 중 미세플라스틱 분석법에 관한 고찰 (The review on standard method of microplastics in soil and groundwater)

  • 권종범;최현희;박선화
    • 분석과학
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    • 제37권3호
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    • pp.174-188
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    • 2024
  • 본 연구에서는 토양 및 지하수 중 미세플라스틱(MP) 분석법 표준화를 위해 관련 국내·외 연구동향을 검토하고 매체 별 시료채취 방법, 전처리 방법 및 분석 장치의 종류 등에 관한 대표적인 방법을 리뷰하였다. 토양 시료채취는 시료채취 지점선정, 채취 깊이 및 시료량을 고려하고 있으며 대부분 15 cm 이내(표토) 깊이에서 약 1 kg의 시료를 혼합채취하는 것으로 파악되었다. 지하수 시료채취는 정치방법과 연속흐름방법 중 연속흐름방식이 대표적이고 채취량 300~1,000 L 구간에서 유량 2~6 L/min로 채취하며 현장 여과하였다. 처리 방법은 두 매체에 공통적으로 유기물 분해와 밀도차 분리로 나뉘며 유기물 분해방법인 H2O2, 산, 알칼리, 효소 활용 중 H2O2가 추천된다. 밀도 분리는 NaCl, ZnCl2, ZnBr2 등의 시약 중 NaCl이 주로 사용되나 분석하고자 하는 MP의 밀도에 따라 시약을 선택적으로 활용할 수 있다. 분석 기기는 비파괴적 분석법인 FTIR, Raman과 파괴 분석법인 Py-GC/MS가 대표적이다. µ-FTIR은 직경 10 ㎛ 이상 Raman은 1 ㎛ 이상의 MP 재질과 개수 분석이 가능하나 전처리를 통해 유기물과 같은 분광분석의 방해요소를 충분히 제거해야 한다. Py-GC/MS는 복잡한 전처리가 필요 없고 특정 재질의 정량분석이 가능하여 지속적으로 연구되어지고 있다.

Electrodeposition of Ternary CdZnS Semiconductor Thin Films Using a S-Modified Polycrystalline Au Electrode

  • Ham, Sun-Young;Cho, Se-Jin;Lee, Ung-Ki;Jeon, So-Yeon;Shin, Ji-Cheol;Myung, No-Seung;Paeng, Ki-Jung
    • 전기화학회지
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    • 제10권4호
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    • pp.262-264
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    • 2007
  • This paper describes a two-step approach for the electrochemical deposition of CdZnS thin films on the polycrystalline Au electrode. Initially, an Au substrate is electrochemically modified with a sulfur layer. In the second step, the layer is electroreduced to $S^{2-}$ in the electrolyte dosed with the requisite amount of $Cd^{2+}$ and $Zn^{2+}$ ions to generate CdZnS films in situ. This approach was validated using a combination of linear sweep voltammetry and electrochemical quartz crystal microgravimetry. Thus synthesized CdZnS thin films have different composition depending on the composition of electrolytes. CdZnS thin films are characterized by energy-dispersive X-ray analysis and Raman spectroscopy.

아크 방전법으로 성장된 대면적 단일벽 탄소나노튜브 필름 (Single Wall Carbon Nanotube Films Produced by Arc Discharge)

  • 강영진;오동훈;송혜진;정진연;정혁;조유석;김도진
    • 한국재료학회지
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    • 제18권5호
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    • pp.253-258
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    • 2008
  • A simple method to deposit carbon nanotube films uniformly on large area substrates using an arc discharge method is reported in this paper. The arc discharge method was modified to deposit carbon nanotube films in situ on the substrates. The substrates were scanned several times over the arcing point for a uniform film thickness. Deposition was carried out under variable dc bias conditions at 600 torr of $H_2$ gas. The thickness uniformity of the single-wall carbon nanotube films as characterized by a four-point probe was within 30% deviation. The morphology and crystal quality of the single-wall carbon nanotube film were also characterized by field emission scanning electron microscopy and Raman spectroscopy.

Sensing characteristics of Polypyrrole-based methanol sensors preparedbyin-situ vapor state polymerization

  • Linshu Jiang;Jun, Hee-Kwon;Hoh, Yong-Su;Lee, Duk-Dong;Huh, Jeung-Soo
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2003년도 춘계학술발표강연 및 논문개요집
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    • pp.137-137
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    • 2003
  • Conducting PPy/PVA composite and pure PPy gas sensors were prepared by in-situ vaporstate polymerization method in a vaporization chamber under N2 condition, by exposing the pre-coated electrode with PVA/FeC13 to distilled pyrrole monomer. The various electrical sensing behaviors of both types of sensors were systematically investigated by a flow measuring system including mass flow controller (MFC) and bubbling bottle. The FT-Raman spectroscopy of vapor state polymerized PPy was identical to that of chemically polymerized PPy, confirming the same chemical structure. Both types of sensors had positive sensitivity when exposed to methanol gas. The sensitivity varied linearly with gas concentration in the range of 50ppm to 1059ppm. The detection limit of PPy/PVA sensor was believed to be as low as 10ppm. The sensitivity of PPy/PVA composite sensor was higher than that of pure PPy sensor. Both the response time and recovery time of PPy/PVA composite sensors were longer than those of pure PPy sensors. The thickness of the sensing film affected the sensitivity this way that the sensor having thinner film had higher sensitivity, indicating that the resistance of polymer film involved in the sensing behavior was bulk resistance rather than surface resistance. The reproducibility of PPy/PVA composite sensor was excellent during eight on-off cycles by switching between N2 and 3000ppm methanol gas. The sensitivity of PPy/PVA composite sensor was only maintained for two weeks, while the sensitivity of pure PPy sensor was maintained over two months.

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Facile in situ Formation of CuO/ZnO p-n Heterojunction for Improved H2S-sensing Applications

  • Shanmugasundaram, Arunkumar;Kim, Dong-Su;Hou, Tian Feng;Lee, Dong Weon
    • 센서학회지
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    • 제29권3호
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    • pp.156-161
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    • 2020
  • In this study, hierarchical mesoporous CuO spheres, ZnO flowers, and heterojunction CuO/ZnO nanostructures were fabricated via a facile hydrothermal method. The as-prepared materials were characterized in detail using various analytical methods such as powder X-ray diffraction, micro Raman spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, and transmission electron microscopy. The obtained results are consistent with each other. The H2S-sensing characteristics of the sensors fabricated based on the CuO spheres, ZnO flowers, and CuO/ZnO heterojunction were investigated at different temperatures and gas concentrations. The sensor based on ZnO flowers showed a maximum response of ~141 at 225 ℃. The sensor based on CuO spheres exhibited a maximum response of 218 at 175 ℃, whereas the sensor based on the CuO/ZnO nano-heterostructure composite showed a maximum response of 344 at 150 ℃. The detection limit (DL) of the sensor based on the CuO/ZnO heterojunction was ~120 ppb at 150 ℃. The CuO/ZnO sensor showed the maximum response to H2S compared with other interfering gases such as ethanol, methanol, and CO, indicating its high selectivity.

리튬이온 전지용 바이오매스 기반 음극재 개발 (Development of Biomass-Derived Anode Material for Lithium-Ion Battery)

  • 정재윤;이동준;허정원;임두현;서양곤;안주현;최창호
    • 청정기술
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    • 제26권2호
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    • pp.131-136
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    • 2020
  • 기존의 석유계부산물 기반 음극재의 대체물질을 개발하고자, 친환경적이며 가격이 저렴한 대나무 기반 1차 탄화숯을 저온 흑연화 공정을 통해 흑연으로 전환 후 음극재로 활용하였다. 저온 흑연화 공정을 위해 탄화철을 촉매로 사용하였으며, 첨가된 탄화철의 양에 따라 흑연화 정도를 X선 회절기(x-ray diffraction, XRD), 라만 분광기(raman spectroscopy), TEM (transmission electron microscopy)을 사용하여 분석 한 후 탄화철의 최적 양을 결정하였다. 가스흡착법(brunauer-emmett-teller, BET)를 사용하여 흑연화 숯의 기공특성도 분석하였다. 분석 결과 촉매 표면을 중심으로 비정질의 탄소가 흑연으로 전환되었으며, 흑연화 공정 후 촉매를 제거하기 위해 산 처리를 하는 동안 기존의 1차 탄화숯보다 크기가 큰 기공이 형성되어 상대적으로 표면적이 줄어들었다. 최적 양의 촉매를 사용하여 제조된 흑연화 숯을 음극재로 활용하여 전지성능을 분석한 결과 1차 탄화숯과 비교하여 방전용량과 충방전 효율이 증가하였다. 이는 흑연화 공정으로 비정질의 탄소가 흑연으로 전환되었기 때문으로 추정되며, 전지성능을 더욱 향상시키기 위해서는 탄화철 촉매의 크기를 최대한 작게 조절하고, 흑연화 숯의 입자크기를 균일화 하는 연구가 필요할 것으로 사료된다.

PECVD를 이용한 2차원 이황화몰리브데넘 박막의 저온합성법 개발

  • 김형우;안치성;;이창구;김태성
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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    • pp.274-274
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    • 2014
  • 금속칼코게나이드 화합물중 하나인 $MoS_2$는 초저 마찰계수의 금속성 윤활제로 널리 사용되고 있으며 흑연과 비슷한 판상 구조를 지니고 있어 기계적 박리법을 통한 그래핀의 발견 이후 2차원 박막 합성법에 대한 활발한 연구가 진행되고 있다. 최근 다양한 응용이 진행 중인 그래핀의 경우 높은 전자이동도, 기계적 강도, 유연성, 열전도도 등 뛰어난 물리적 특성을 지니고 있으나 zero-bandgap으로 인한 낮은 on/off ratio는 thin film transistor (TFT), 논리회로(logic circuit) 등 반도체 소자 응용에 한계가 있다. 하지만 $MoS_2$는 벌크상태에서 약 1.2 eV의 indirect band-gap을 지닌 반면 단일층의 경우 1.8 eV의 direct-bandgap을 나타내고 있다. 또한 단일층 $MoS_2$를 이용하여 $HfO_2/MoS_2/SiO_2$ 구조의 트랜지스터를 제작하였을 때 $200cm^2/v^{-1}s^{-1}$의 높은 mobility와 $10^8$ 이상의 on/off ratio 나타낸다는 연구가 보고되어 있어 박막형 트랜지스터 응용을 위한 신소재로 주목을 받고 있다. 한편 2차원 $MoS_2$ 박막을 합성하기 위한 대표적인 방법인 기계적 박리법의 경우 고품질의 단일층 $MoS_2$ 성장이 가능하지만 대면적 합성에 한계를 지니고 있으며 화학기상증착법(CVD)의 경우 공정 gas의 분해를 위한 높은 온도가 요구되므로 박막형 투명 트랜지스터 응용을 위한 플라스틱 기판으로의 in-situ 성장이 어렵기 때문에 이를 보완할 수 있는 $MoS_2$ 박막 합성 공정 개발이 필요하다. 특히 Plasma enhanced chemical vapor deposition (PECVD) 방법은 공정 gas가 전기적 에너지로 분해되어 chamber 내부에서 cold-plasma 형태로 존 재하기 때문에 박막의 저온성장 및 대면적 합성이 가능하며 고진공을 바탕으로 합성 중 발생하는 오염 요소를 효과적으로 제어할 수 있다. 본 연구에서는PECVD를 이용하여 plasma power, 공정압력, 공정 gas의 유량 등 다양한 공정 변수를 조절함으로써 저온, 저압 조건하에서의 $MoS_2$ 박막 성장 가능성을 확인하였으며 전구체로는 Mo 금속과 $H_2S$ gas를 사용하였다. 또한 향후 flexible 소자 응용을 위한 플라스틱 기판의 녹는점을 고려하여 공정 온도는 $300^{\circ}C$ 이하로 설정하였으며 합성된 $MoS_2$ 박막의 두께 및 화학적 구성은 Raman spectroscopy를 이용하여 확인 하였다. 공정온도 $200^{\circ}C$$150^{\circ}C$에서 성장한 $MoS_2$ 박막의 Raman peak의 경우 상대적으로 낮은 공정온도로 인하여 Mo와 H2S의 화학적 결합이 감소된 것을 관찰할 수 있었고 $300^{\circ}C$의 경우 약 $26{\sim}27cm^{-1}$의 Raman peak 간격을 통해 5~6층의 $MoS_2$ 박막이 형성 된 것을 확인할 수 있었다.

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Salinity Effect on the Equilibria and Kinetics of the Formation of CO2 and R-134a Gas Hydrates in Seawater

  • Johanna, Lianna;Kim, A Ram;Jeong, Guk;Lee, Jea-Keun;Lee, Tae Yun;Lim, Jun-Heok;Won, Yong Sun
    • 한국재료학회지
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    • 제26권7호
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    • pp.382-387
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    • 2016
  • Gas hydrates are crystalline solids in which gas molecules (guests) are trapped in water cavities (hosts) that are composed of hydrogen-bonded water molecules. During the formation of gas hydrates in seawater, the equilibria and kinetics are then affected by salinity. In this study, the effects of salinity on the equilibria of $CO_2$ and R134-a gas hydrates has been investigated by tracing the changes of operating temperature and pressure. Increasing the salinity by 1.75% led to a drop in the equilibrium temperature of about $2^{\circ}C$ for $CO_2$ gas hydrate and $0.38^{\circ}C$ for R-134a gas hydrate at constant equilibrium pressure; in other words, there were rises in the equilibrium pressure of about 1 bar and 0.25 bar at constant equilibrium temperature, respectively. The kinetics of gas hydrate formation have also been investigated by time-resolved in-situ Raman spectroscopy; the results demonstrate that the increase of salinity delayed the formation of both $CO_2$ and R134-a gas hydrates. Therefore, various ions in seawater can play roles of inhibitors for gas hydrate formation in terms of both equilibrium and kinetics.

Structural Evolution of Layered $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ upon Electrochemical Cycling in a Li Rechargeable Battery

  • 홍지현;서동화;김성욱;권혁조;박영욱;강기석
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2010년도 춘계학술발표대회
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    • pp.37.2-37.2
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    • 2010
  • Recently $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ has been consistently examined and investigated by scientists because of its high lithium storage capacity, which exceeds beyond the conventional theoretical capacity based on conventional chemical concepts. Consequently, $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ is considered as one of the most promising cathode candidates for next generation in Li rechargeable batteries. Yet the mechanism and the origin of the overcapacity have not been clarified. Previously, many authors have demonstrated simultaneous oxygen evolution during the first delithiation. However, it may only explain the high capacity of the first charge process, and not of the subsequent cycles. In this work, we report a clarified interpretation of the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$, which is the key element in understanding its anomalously high capacity. We identify how the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ occurs upon the electrochemical cycling through careful study of electrochemical profiles, ex-situ X-ray diffraction (XRD), HR-TEM, Raman spectroscopy, and first principles calculation. Moreover, we successfully separated the structural change at subsequent cycles (mainly cation rearrangement) from the first charge process (mainly oxygen evolution with Li extraction) by intentionally synthesizing sample with large particle size. Consequently, the intermediate states of structural evolution could be well resolved. All observations made through various tools lead to the result that spinel-like cation arrangement and lithium environment are created and embedded in layered framework during repeated electrochemical cycling.

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