• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.35 no.5
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• pp.431-438
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• 2022

In functional materials, in situ experimental techniques as a function of external stimulus (e.g., electric field, magnetic field, light, etc.) or changes in ambient environments (e.g., temperature, humidity, pressure, etc.) are highly essential for analyzing how the physical properties of target materials are activated/evolved by the given stimulation. In particular, in situ electric-field-dependent X-ray diffraction (XRD) measurements have been extensively utilized for understanding the underlying mechanisms of the emerging electromechanical responses to external electric field in various ferroelectric, piezoelectric, and electrostrictive materials. This tutorial article briefly introduces basic principles/key concepts of in situ electric-field-dependent XRD analysis using a lab-scale XRD machine. We anticipate that the in situ XRD method provides a practical tool to systematically identify/monitor a structural modification of various electromechanical materials driven by applying an external electric field.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.181-181
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• 2013

Recently, nanostructure and the molecular orientation of organic thin films have been largely paid attention due to its importance in organic electronics such as organic thin film transistors (OTFTs), organic light emitting diodes (OLEDs), and organic photovoltaics (OPVs). Among various methods, the diffraction and scattering techniques based on synchrotron x-rays have shown powerful results in organic thin film systems. In this work, we introduce the in-situ annealing system installed at PLS-II (Pohang Light Source II) for organic thin films by simultaneously conducting various x-ray scattering measurements of x-ray reflectivity, conventional x-ray scattering, grazing incidence wide angle x-ray scattering (GI-WAXS) and so on. Using the in-situ measurement, we could obtain real time variation of nanostructure as well as molecular orientation during thermal annealing in metal-phthalocyanine thin films. The variation of surface and interface also could be simultaneously investigated by the x-ray reflectivity measurement.

• Ceramist
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• v.22 no.4
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• pp.402-416
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• 2019

The development of next-generation secondary batteries, including lithium-ion batteries (LIB), requires performance enhancements such as high energy/high power density, low cost, long life, and excellent safety. The discovery of new materials with such requirements is a challenging and time-consuming process with great difficulty. To pursue this challenging endeavor, it is pivotal to understand the structure and interface of electrode materials in a multiscale level at the atomic, molecular, macro-scale during charging / discharging. In this regard, various advanced material characterization tools, including the first-principle calculation, high-resolution electron microscopy, and synchrotron-based X-ray techniques, have been actively employed to understand the charge storage- and degradation-mechanisms of various electrode materials. In this article, we introduce and review recent advances in in-situ synchrotron-based x-ray techniques to study electrode materials for LIBs during thermal degradation and charging/discharging. We show that the fundamental understanding of the structure and interface of the battery materials gained through these advanced in-situ investigations provides valuable insight into designing next-generation electrode materials with significantly improved performance in terms of high energy/high power density, low cost, long life, and excellent safety.

• Economic and Environmental Geology
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• v.45 no.2
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• pp.79-88
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• 2012

The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

• Corrosion Science and Technology
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• v.7 no.2
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• pp.112-118
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• 2008

We observed initial rusting process of steel containing Al under wet/dry cyclic condition with NaCl solution film using in situ X-ray diffraction spectroscopy at SPring-8 synchrotron radiation facility. It was found that mass fraction of iron oxides such as ${\alpha}-FeOOH$, ${\beta}-FeOOH$ and ${\gamma}-FeOOH$ varied with Al content. Some kinds of Al oxides were also found at the initial stage of corrosion. Those corrosion products might affect the corrosion process and corrosion rate of the steel.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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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.

• Proceedings of the Korean Magnestics Society Conference
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• 2009.12a
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• pp.204-205
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• 2009

The magnetic properties and structure of FeRh thin film pitaxially grown onto MgO(001) substrate were studied by MPMS(Magnetic Properties Measure System) and in-situ temperature synchrotron XRD(X-ray Diffraction). The transition temperature of FeRh thin films was around 380K. Both M-T curve and d-spacing changes correspond to each other very closely.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2019.05a
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• pp.149-150
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• 2019

• Journal of the Korean Vacuum Society
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• v.10 no.1
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• pp.22-26
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• 2001

Microstructures of AlN thin films on Si substrates grown by plasma assisted molecular beam epitaxy were analyzed with various growth temperatures and substrate orientations. Reflection high energy electron diffraction (RHEED) patterns were checked for the in-situ monitoring of the growth condition. X-ray diffraction(XRD), double crystal X-ray diffraction (DCXD), and transmission electron microscopy/diffraction (TEM/TED) techniques were employed to characterize the microstructure of the films after growth. On Si(100) sub-strates, AlN thin films were grown mostly along the hexagonal c-axis orientation at temperature higher than $850^{\circ}C$. On the other hand the AlN films on Si(111) were epitaxially grown with directional coherencies in AlN(0001)/Si(111), AlN(1100)/Si(110), and AlN(1120)/Si(112). The microstructure of AlN thin films on Si(111) substrates, with a full width at half maximum of almost 3000 arcsec at 2$\theta$=$36.2^{\circ}$, showed that the single crystal films were grown, even if they includ a lot of crystal defects such as dislocations and stacking faults.

• Journal of Electrochemical Science and Technology
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• v.3 no.1
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• pp.29-34
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• 2012

The structural changes of $Li_{1-x}Ni_{0.5}Co_{0.2}Mn_{0.3}O_2$ cathode material for lithium ion battery during the first charge was investigated in comparison with $Li_{1-x}Ni_{0.8}Co_{0.15}Al_{0.05}O_2$ using a synchrotron based in situ X-ray diffraction technique. The structural changes of these two cathode materials show similar trend during first charge: an expansion along the c-axis of the unit cell with contractions along the a- and b-axis during the early stage of charge and a major contraction along the c-axis with slight expansions along the a- and b-axis near the end of charge at high voltage limit. In $Li_{1-x}Ni_{0.5}Co_{0.2}Mn_{0.3}O_2$ cathode, however, the initial unit cell volume of H2 phase is bigger than that of H1 phase since the c-axis undergo large expansion while a- and b- axis shrink slightly. The change in the unit cell volume for $Li_{1-x}Ni_{0.5}Co_{0.2}Mn_{0.3}O_2$ during charge is smaller than that of $Li_{1-x}Ni_{0.8}Co_{0.15}Al_{0.05}O_2$. This smaller change in unit cell volume may give the $Li_{1-x}Ni_{0.5}Co_{0.2}Mn_{0.3}O_2$ cathode material a better structural reversibility for a long cycling life.