• 폴리머
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• 제29권1호
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• pp.87-90
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• 2005

본 연구에서는 폴리스티렌/점토 나노복합재료를 스티렌 단량체를 이용한 in-situ 중합법으로 제조하면서, 여러가지 유기화제로 처리한 점토들의 박리거동을 실시간 XRD 분석을 통해 확인하였다. 실시간 XRD 실험은 포항 가속기 연구소의 4CI 빔라인에서 수행되었다. 사용된 점토의 양이온 교환능과 유기화제의 구조에 의해서 서로 다른 박리거동을 보여주었다. 양이온교환능이 높은 10A-MMT와 15A-MMT의 경우, 스티렌 단량체의 중합과정중 점토의 특성피크 위치는 변화가 없었다. 하지만, 양이온교환능이 상대적으로 낮고 벤질그룹 혹은 비닐그룹을 포함하고 있는 점토들(25A-MMT와 VDAC-MMT)의 경우, 중합초기 점토의 특성피크가 중합시간이 증가함에 따라 점진적으로 저각도쪽으로 움직이며 점토층간 박리현상이 진행되는 것을 확인하였다.

• Nuclear Engineering and Technology
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• 제56권2호
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• pp.402-409
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• 2024

High energy neutron irradiations impact on structural and electrical properties of alumina are studied with particular emphasis on real time in-situ radiation induced conductivity measurement in low flux region. Polycrystalline Al₂O₃ samples are subjected to high energy neutrons produced from D-T neutron generator and Am-Be neutron source. 14 MeV neutrons from D-T generator are chosen to study the role of fast neutron irradiation in the structural modification of samples. Real time in-situ electrical measurement is performed to investigate the change in insulation resistance of Al₂O₃ due to radiation induced conductivity at low flux regime. During neutron irradiation, a significant transient decrease in insulation resistance is observed which recovers relative higher value just after neutron exposure is switched off. XRD results of 14 MeV neutron irradiated samples suggest annealing effect. Impact of relatively low energy neutrons on the structural properties is also studied using Am-Be neutrons. In this case, clustering is observed on the sample surface after prolonged neutron exposure. The structural characterizations of pristine and irradiated Al₂O₃ samples are performed using XRD, SEM, and EDX. The results from these characterizations are analysed and interpreted in the manuscript.

• 대한금속재료학회지
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• 제49권1호
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• pp.46-51
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• 2011

Real-time formation of $L1_0$ phase of FePt nanoparticles in the gas phase during ultrasonic-spray pyrolysis is first discussed in the present study. Without any post heat treatment, $L1_0$ phase of FePt nanoparticles appeared at the temperature above $900^{\circ}C$ in the gas phase synthesis. X-ray diffractometry (XRD) and transmission electron microscopy (TEM) studies revealed that FePt nanoparticles less than 10 nm in size contained small volume of $L1_0$ fct phase. However, in other samples obtained at the temperature below $900^{\circ}C$, iron oxide phase co-existed and no evidence of phase transformation was found. Thus, it is anticipated that the time of flight of particles required for crystallization and phase transformation was extended according to the increase of the collision rate. Finally, magnetic properties represented by coercivity and saturation magnetization and functional groups on the particle surface were discussed based on VSM and FT-IR results.

• 한국전기전자재료학회논문지
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• 제32권1호
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• pp.64-69
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• 2019

Methylammonium lead triiodide ($MAPbI_3$)-based perovskite solar cells potentially have potential advantages such as high efficiency and low-cost manufacturing procedures. However, $MAPbI_3$ is structurally unstable and has low phase-change temperatures ($30^{\circ}C$ and $130^{\circ}C$); it is necessary to solve these problems. We investigated the crystal structure and phase separation using real-time temperature-change X-ray diffraction, transmission electron microscopy, and electron energy loss spectroscopy. $MAPbI_3$ has a tetragonal structure, and at about $35^{\circ}C$ the c-axis contracts, transforming $MAPbI_3$ into the related cubic crystal structure. In addition, at $130^{\circ}C$, phase separation occurs in which $CH_3NH_2$ and HI at the center of the unit cell of the perovskite structure are extracted by gas, leavingand only $PbI_2$ of the three-component structure, is produced as the final solid product.

• 한국입자에어로졸학회지
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• 제17권1호
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• pp.1-8
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• 2021

The purpose of this study is to assess respirable crystalline silica (RCS) exposure levels in workers who collect and dispose used coal briquette ash (CBA) in sanitation companies that are subcontracted by one medium-sized local government on the collection of municipal household waste (MHW), and to analyze the quartz content in CBA. When the CBA powder that undergone specialized pretreatment in several steps were subjected to mineral identification and quantitative analysis using X-ray diffraction (XRD), it was found that quartz represented 18%, and in addition, mullite, and plagioclase were included. For two CBA collectors, samples were collected by the personal sampling evaluation method. After respirable dust was collected in accordance with the National Institute for Occupational Safety and Health 7500 method, the concentration of quartz was analyzed using XRD. Meanwhile, a portable real-time dust monitor (Sidepak AM520, TSI Inc., USA) was also used to observe the dust exposure level for each time zone and job task. The RCS exposure level of one worker was as high as 0.024 mg/㎥, which was the American Conference of Governmental Industrial Hygienists (ACGIH) Threshold Limit Values (TLV) level. The other worker also exhibited a concentration of 0.013 mg/㎥, which was more than half of TLV. The Sidepak results revealed that the work of collecting CBA and loading it onto a vehicle was hardly exposed to the dust of a significant level. It was found, however, that the work of transferring the collected CBA to a container through a conveyor belt was exposed to a very high average respirable dust concentration of 2.238 mg/㎥. The results of this study confirmed that quartz, which is crystalline silica and a carcinogen, is contained in CBA, one of municipal household waste (MHW), in high concentration. It was also confirmed that workers are exposed to high RCS concentrations while transferring collected CBA into a container. Although each local government in South Korea handles CBA in different ways, it is imperative to investigate the CBA exposure level of sanitation workers and improve their working conditions.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2011년도 춘계학술발표대회
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• pp.5-5
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• 2011

The research and development of hybrid electric vehicle (HEV), plug-in hybrid electric vehicle (PHEV) and electric vehicle (EV) are intensified due to the energy crisis and environmental concerns. In order to meet the challenging requirements of powering HEV, PHEV and EV, the current lithium battery technology needs to be significantly improved in terms of the cost, safety, power and energy density, as well as the calendar and cycle life. One new technology being developed is the utilization of composite cathode by mixing two different types of insertion compounds [e.g., spinel $LiMn_2O_4$ and layered $LiMO_2$ (M=Ni, Co, and Mn)]. Recently, some studies on mixing two different types of cathode materials to make a composite cathode have been reported, which were aimed at reducing cost and improving self-discharge. Numata et al. reported that when stored in a sealed can together with electrolyte at $80^{\circ}C$ for 10 days, the concentrations of both HF and $Mn^{2+}$ were lower in the can containing $LiMn_2O_4$ blended with $LiNi_{0.8}Co_{0.2}O_2$ than that containing $LiMn_2O_4$ only. That reports clearly showed that this blending technique can prevent the decline in capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and related structural phase transitions for these composite cathodes. In this presentation, we will report our in situ x-ray diffraction studies on this mixed composite cathode material during charge-discharge cycling. The mixed cathodes were incorporated into in situ XRD cells with a Li foil anode, a Celgard separator, and a 1M $LiPF_6$ electrolyte in a 1 : 1 EC : DMC solvent (LP 30 from EM Industries, Inc.). For in situ XRD cell, Mylar windows were used as has been described in detail elsewhere. All of these in situ XRD spectra were collected on beam line X18A at National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory using two different detectors. One is a conventional scintillation detector with data collection at 0.02 degree in two theta angle for each step. The other is a wide angle position sensitive detector (PSD). The wavelengths used were 1.1950 ${\AA}$ for the scintillation detector and 0.9999 A for the PSD. The newly installed PSD at beam line X18A of NSLS can collect XRD patterns as short as a few minutes covering $90^{\circ}$ of two theta angles simultaneously with good signal to noise ratio. It significantly reduced the data collection time for each scan, giving us a great advantage in studying the phase transition in real time. The two theta angles of all the XRD spectra presented in this paper have been recalculated and converted to corresponding angles for ${\lambda}=1.54\;{\AA}$, which is the wavelength of conventional x-ray tube source with Cu-$k{\alpha}$ radiation, for easy comparison with data in other literatures. The structural changes of the composite cathode made by mixing spinel $LiMn_2O_4$ and layered $Li-Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ in 1 : 1 wt% in both Li-half and Li-ion cells during charge/discharge are studied by in situ XRD. During the first charge up to ~5.2 V vs. $Li/Li^+$, the in situ XRD spectra for the composite cathode in the Li-half cell track the structural changes of each component. At the early stage of charge, the lithium extraction takes place in the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component only. When the cell voltage reaches at ~4.0 V vs. $Li/Li^+$, lithium extraction from the spinel $LiMn_2O_4$ component starts and becomes the major contributor for the cell capacity due to the higher rate capability of $LiMn_2O_4$. When the voltage passed 4.3 V, the major structural changes are from the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, while the $LiMn_2O_4$ component is almost unchanged. In the Li-ion cell using a MCMB anode and a composite cathode cycled between 2.5 V and 4.2 V, the structural changes are dominated by the spinel $LiMn_2O_4$ component, with much less changes in the layered $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, comparing with the Li-half cell results. These results give us valuable information about the structural changes relating to the contributions of each individual component to the cell capacity at certain charge/discharge state, which are helpful in designing and optimizing the composite cathode using spinel- and layered-type materials for Li-ion battery research. More detailed discussion will be presented at the meeting.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2007년도 추계학술대회 논문집
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• pp.28-28
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• 2007

Ferroelectric $(Ba_{0.5}Sr_{0.5})TiO_3$ (BST) thin films of thickness 500nm were deposited on $LaAlO_3$, (LAO) substrates by at $800^{\circ}C$. BST films were characterized for structure using X-ray diffraction (XRD). The surface morphology and thickness of BST the films were characterized by atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM). We measured the dielectric properties at microwave frequencies (1~3 GHz) using a symmetrical stripline resonator with shorted ends and terahertz frequencies (0.2~2.5 THz) using a time-domain terahertz spectroscopy. The real and imaginary parts of the complex dielectric constant of the BST thin films on LAO substrates were in agreement with those previously reported.

• 자원환경지질
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• 제51권4호
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• pp.359-370
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• 2018

기존 연구에서 초임계$CO_2$($scCO_2$)-물-순활골재 반응을 이용한 폐콘크리트 순환골재의 중성화(pH 저감) 처리에서 가장 문제시되었던 오랜 처리시간의 한계(최대 50일)를 최소 3시간까지 단축하는 배치실험과 칼럼실험을 수행하였다. 모르타르(골재를 포함하지 않은 시멘트+모래 혼합체)와 모르타르에 골재를 포함하는 2 종류의 순환골재를 실험에 사용하였다. 입자 크기별로 분류한 세 종류의 폐모르타르 시료에 대하여 $scCO_2$-물-폐모르타르 반응 시간을 1시간부터 24시간까지 다하게 설정하여 반응시킨 후, 폐모르타르의 pH가 지속적으로 9.8 이하로 낮게 유지되는 최소 반응시간을 결정하는 용출 배치실험을 실시하였다. 실제 현장에서 다량의 순환골재를 중성화 처리하는 경우 비평형상태에서 용출이 발생하는데, 이러한 kinetic 효과를 고려한 순환골재의 실제 pH 저감 효율을 측정하고자 대형 칼럼 연속 용출 실험을 실시하였다. 배치실험의 경우, 고압셀 내부에서 3차 증류수 70 mL와 순환골재 시료 35 g을 혼합한 후 100 bar, $50^{\circ}C$ 조건에서 1시간 ~ 24시간 동안 반응시켜 중성화 처리하였다. 처리 후 건조시킨 폐모르타르 시료 10 g + 증류수 50 ml의 비율(1:5 비율)로 혼합하여 10분 동안 150 rpm으로 교반한 후 정치시키고, 총 15일 동안 용출시간 별로 용출수의 pH를 측정하였다. 중성화 처리 후 순환골재의 광물학적 변화를 확인하기 위하여 처리 전/후 XRD, TG/DTA 등의 분석을 실시하였다. 대형 칼럼(직경 16 cm, 높이 1 m) 용출실험을 위해 순환골재 2 종류를 대상으로 3시간 동안 중성화 처리한 순환골재와 처리하지 않은 순환골재로 칼럼을 충진한 후, 증류수를 칼럼 상부에 설치된 스프링클러를 통하여 일정하게 총 220 L를 주입하였다. 칼럼에 충진된 순환골재를 통과하여 하부로부터 유출되는 유출수의 pH와 $Ca^{2+}$ 농도를 시간별로 측정하였다. 배치실험 결과 폐모르타르 시료(직경 10 ~ 13 mm)의 경우 3시간의 중성화 처리에 의해 용출액의 pH가 법적 허용기준인 9.8이하를 유지하는 것으로 나타났다. $scCO_2$ 반응 후 골재의 XRD, TG/DTA 분석 결과, 중성화 처리에 의해 시멘트 모르타르의 주성분인 포틀랜다이트($Ca(OH)_2$) 성분이 감소한 반면 방해석($CaCO_3$)이 2차 광물로 생성됨을 알 수 있었다. 칼럼 실험 결과 중성화 처리한 순환골재의 용출수는 kinetic 효과를 고려한 경우에도 굵은골재와 잔골재 모두 용출수의 pH가 9.8 이하로 유지되어, $scCO_2$를 이용한 순환골재의 3시간 중성화 처리에 의해 건설현장에서 재활용이 가능한 것으로 밝혀졌다.

• Advances in nano research
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• 제13권6호
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• pp.513-525
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• 2022

In this study, it was aimed to evaluate direct oxidation of aqueous solution containing cefalexin antibiotic with new generation Sn/Sb/Ni: 500/8/1 anode. The fact that there is no such a study on treatment of cefalexin with these new anode made this study unique. According to the operating parameters evaluation COD graphs showed clearer results compared to TOC and CLX and thus, it was it was chosen as major parameter. Furthermore, pseudo-first degree kd values were calculated from CLX results to show more accurate and specific results. Experimental results showed that after 60 min of electrochemical oxidation, complete removal of COD and TOC was accomplished with 750 mg L^-1 KCl, at pH 7, 50 mA cm^-2 current density and 1 cm anode-cathode distance. Also, the stability of the Sn/Sb/Ni anode was evaluated by taking SEM and AFM images and XRD analysis before and after of electrochemical oxidation processes. According to the results, it was not occurred too much change on the anode surface even after 300 h of electrolysis. Thus, it was thought that the anode material was not corroded to a large extent. Furthermore, the removal efficiencies were very high for almost all the time and conditions. According to the results of the study, electrochemical oxidation with new generation Sn/Sb/Ni anodes for the removal of cefalexin antibiotic was found very successful and applicable due to require less reaction time complete mineralization and doesn't require pH adjustment step compared to other studies in literature. In future studies, different antibiotic types should be studied with this anode and maybe with real wastewaters to test applicability of the process in treatment of pharmaceutical wastewaters containing antibiotics, in a better way.

• 자원환경지질
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• 제50권4호
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• pp.257-266
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• 2017

본 연구에서는 초임계 $CO_2$($scCO_2$)를 이용하여 폐콘크리트 순환골재와 반응한 용출수의 pH를 9.8 이하로 유지시켜(중성화) 재활용할 수 있는 기술을 개발하기 위한 실내 배치실험을 수행하였다. 실험재료로는 건설폐기물중간처리업체에서 제공받은 세 종류의 순환골재를 사용하였으며, 각 종류별로 골재 입자크기 별로 선별하여 총 7개의 시료를 사용하였다. 먼저 $scCO_2$-물-순환골재 반응에 의해 순환골재의 pH가 지속적으로 낮게 유지되는지를 확인하는 반응실험을 수행하였다. 스테인레스강철로 만들어진 고압셀(150 mL 용량)에 테플론 비이커를 고정시킨 후, 3차 증류수 70 mL와 순환골재 시료 35 g을 혼한한 후 고압용 오븐과 고압시린지 펌프 및 압력조절 장치를 이용하여 10 MPa(100 bar), $50^{\circ}C$ 조건에서 50일간 반응시켰다. 반응시간(1, 5, 10, 15, 30, 50일)에 따른 증류수의 pH, 용존 양이온과 음이온 농도를 측정하였다. $scCO_2$ 반응에 의한 순환골재의 지화학적 및 광물학적 변화를 확인하기 위하여 반응 전/후 XRD, SEM-EDS 등의 분석을 실시하였다. 마지막으로 $scCO_2$ 반응 후 순환골재의 용출수 pH 변화를 용출실험을 통하여 규명하였다. $scCO_2$-물-순환골재 반응 결과, 반응 전 순환골재의 pH는 평균 12보다 높은 값을 나타내었으나, $scCO_2$와 반응한 지 1시간 경과 후 증류수의 pH는 7이하로 낮아졌고 반응 50일 까지 pH가 8 이하로 안정되게 유지되었다. 순환골재 종류와 관계없이 $scCO_2$와의 용해 반응에 의해 수용액 내 $Ca^{2+}$, $Si^{4+}$, $Mg^{2+}$, $Na^+$ 이온들의 농도가 증가하였으며, $scCO_2$ 반응 후 골재의 XRD, SEM-EDS 분석 결과, 다량의 방해석과 일부 무정형의 규산염과 수산화물이 침전되었다. $scCO_2$로 처리하지 않은 순환골재의 용출수 pH는 용출 시간에 관계없이 12-13을 유지하였으나, $scCO_2$로 50일 처리한 경우와 1일 처리한 순환골재의 경우 모두, 입자크기와 관계없이 용출수의 pH가 9이하를 유지하여 건설현장에서 순환골재의 재활용이 가능할 것으로 판단되었다.