• 한국전기전자재료학회논문지
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• 제35권5호
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• pp.431-438
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• 2022

기능성 소재연구에서 in situ 분석 기법은 외부 자극 (전기장, 자기장, 빛, 등) 또는 주변 환경 (온도, 습도, 압력, 등)과 같이 주어진 자극에 의해 소재의 물리적 특성이 어떻게 활성화/진화되는지 분석하는데 있어서 매우 중요하다. 특히, 전기장 인가에 따른 in situ X-선 회절(XRD) 실험은 다양한 강유전체, 압전체, 전왜 재료의 외부 전기장 인가에 따른 전기-기계적 반응의 기본 원리를 이해하기 위해 광범위하게 활용되었다. 본 튜토리얼 논문에서는 일반 실험실 규모의 XRD 장비를 이용하여 전기장 인가에 따른 in situ XRD 분석의 기본 원리/핵심 개념을 간략하게 소개한다. In situ XRD 측정법은 외부 전기장을 인가하여 구동되는 다양한 전기-기계 재료의 구조적 변형을 체계적으로 식별/모니터링하는 데 매우 유용할 것으로 기대한다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2012년도 춘계학술발표회 논문집
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• pp.210-210
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• 2012

본 연구에서는 터치패널에 적용되는 ITO 박막의 $SnO_2$ 함량별(2, 3, 5, 10wt%) 특성을 확보하기 위하여, Sputtering 장치를 사용하여 ITO 박막을 상온에서 증착한 후 In-situ HT(High temperature)-XRD를 이용하여 온도에 따른 구조적 특성변화를 조사하였다. In-situ HT-XRD 측정 시 온도는 170, 200, $250^{\circ}C$, 유지시간은 1시간으로 제어하였다.

• 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.

• 한국전기전자재료학회논문지
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• 제13권12호
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• pp.1032-1038
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• 2000

Ni$_{81}$$Fe_{19}$(200 nm) thin films have been deposited by RF-magnetron sputtering on Si(001) substrates, Atomic force microscopy(AFM), X-ray diffraction(XRD) and magnetoresistance(MR) measurements of the thin films for investigating electromagnetic properties and microstructures were employed. During field annelaing for 1hr, there was no big difference n XRD patterns of Ni$_{81}$$Fe_{19}$ thin films. However, there was a significant change in XRD patterns of Ni$_{81}$$Fe_{19}$ thin films deposited at 40$0^{\circ}C$ during in-situ magnetic field deposition. The degree of surface roughness increased with increasing annealing and deposition temperature. With variation of surface roughness, there was no significant difference in MR Characteristics of Ni$_{18}$ $Fe_{19}$ thin films in 1hr-annealed case. High MR ratio was observed in the case of in-situ field deposited Ni$_{81}$$Fe_{19}$ films. 19/ films.

• 한국결정성장학회지
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• 제25권5호
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• pp.225-229
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• 2015

본 연구에서는 Mn-Co-Ni 삼성분계로 이루어진 NTC 서미스터의 cubic 스핀넬 결정구조의 변화를 고찰하고자 하였다. Mn, Co, Ni로 이루어진 산화물 원재료 분말들을 혼합하고 건조한 후 In-situ XRD 장비를 이용하여 공기분위기에서 상온부터 $1400^{\circ}C$까지 가열하면서 발생하는 결정구조 변화를 분석하였다. In-situ XRD 분석 결과 cubic 스핀넬 구조는 $900^{\circ}C$부터 존재하는 것을 확인할 수 있었으나, 온도가 $1300^{\circ}C$ 이상으로 올라갔을 때는 스핀넬 결정구조로부터 NiO의 상분리 현상이 발생하기 시작함을 관찰할 수 있었다. 이러한 NiO 상의 분리가 고온에서의 NTC 서미스터의 결정성 감소의 원인임을 알 수 있었으며, 제작된 NTC 서미스터의 표면을 FE-SEM을 이용하여 관찰하여 양품과 불량품의 차이를 분석하였다.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1288-1288
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• 2001

X-ray powder diffraction (XRD) is utilized for determination of polymorphism in crystalline organic materials. Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications. Near-Infrared spectroscopy (NIR) can be adapted to in situ manufacturing schemes by use of a source/detector probe. Conversely, NIR is unable to conclusively define the existence of polymorphism in crystalline materials. By combining the two techniques, a novel simultaneous NIR/XRD instrument has been developed. During material's analysis, results from XRD allow for defining the polymorphic phase present, and NIR data are collected as a fingerprint for each of the observed polymorphs. These NIR fingerprints will allow for the development of a library, which can be referenced during the use of a NIR probe in manufacturing settings.

• 한국전기화학회:학술대회논문집
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• 한국전기화학회 2003년도 춘계총회 및 학술발표회
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• pp.22-22
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• 2003

• 한국재료학회지
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• 제14권5호
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• pp.305-309
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• 2004

Mechanical alloying (MA) of Ti-25.0～37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0～26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1～37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1～37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

• 한국재료학회지
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• 제14권5호
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• pp.310-314
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• 2004

Mechanical alloying (MA) of Ti-50.0～66.7at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-50.0～59.6at%Si powders showed that there were exothermic peaks during MA, indicating TiSi, $TiS_2$, and $Ti_{5}$ $Si_4$ phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). Those of Ti-59.8～66.7 at%Si powders, however, showed that there were no peaks during MA, indicating any Ti silicide was not synthesised until MA 240 min. For Ti-50.0～59.6at%Si powders, the critical milling times for SHS increased from 34.5 min to 89.5 min and the temperature rise, $\Delta$T (=peak temperature-onset temperature) decreased form $26.2^{\circ}C$ to $17.1^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 59.6at% and the critical value of the negative heat of formation of Ti-59.6at%Si to be -1.48 kJ/g.

• 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.