We have studied the thermal stability of NCM622 cathode material for Li-ion batteries using real-time synchrotron x-ray scattering below 600°C in both air and vacuum. The expansion of the mean particle size, which reached maximum values of 10.3 μm in air and 10.6 μm in vacuum at 200°C, was attributed to the dehydration of intergranular water within the NCM622 powders. Across all annealing temperatures, the amount of crystal NCM622 phase in air was consistently higher than that in vacuum. The crystal domain sizes in air showed less variation than that in vacuum during annealing from RT to 500°C. These indicate that the crystal NCM622 phase is more thermally stable during annealing in air than in vacuum. This stability is attributed to the presence of 21% oxygen in air, which is absent under vacuum conditions.
Rietveld refinement has become an essential tool for the quantitative analysis of crystal structures in polycrystalline systems using X-ray diffraction data. This tutorial paper focuses on the background, case studies, and practical implementation of Rietveld refinement using the open-source software PROFEX. Key structural parameters, such as lattice constants and phase fractions, can be quantitatively extracted through full-pattern fitting. Case studies involving compositional variation, electric fields, temperature changes, and battery cycling demonstrate the broad applicability of Rietveld refinement in materials science, energy storage, and catalysis. A step-by-step procedure for performing Rietveld refinement is presented using Bi1/2Na1/2TiO3 perovskite ceramic as an example, providing guidance on software installation, preparing crystal structure information files, performing Rietveld refinement, evaluating results using R-factor and χ² values, and summarizing the results. This tutorial aims to improve understanding and accessibility of Rietveld refinement for researchers seeking to investigate structure-property relationships in complex material systems.
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.
Spectroscopies are the most widely used for understanding the crystallographic, chemical, and physical aspects of materials; therefore, numerous commercial and non-commercial software have been introduced to help researchers better handling their spectroscopic data. However, not many researchers, especially early-stage ones, have a proper background knowledge on the choice of fitting functions and a technique for actual fitting, although the essence of such data analysis is peak fitting. In this regard, we present a practical guide for peak fitting for data analysis. We start with a basic-level theoretical background why and how a certain protocol for peak fitting works, followed by a step-by-step visualized demonstration how an actual fitting is performed. We expect that this contribution is sure to help many active researchers in the discipline of materials science better handle their spectroscopic data.
We fabricated BiAlO thin film by a solution process with a brush coating to be used as liquid crystal (LC) alignment layer. Solution-processed BiAlO was coated on the glass substrate by brush process. Prepared thin films were annealed at different temperatures of 80℃, 180℃, and 280℃. To verify whether the BiAlO film was formed properly, X-ray photoelectron spectroscopy analysis was performed on Bi and Al. Using a crystal rotation method by polarized optical microscopy, LC alignment state was evaluated. At the annealing temperature of 280℃, the uniform homogenous LC alignment was achieved. To reveal the mechanism of LC alignment by brush coating, field emission scanning electron microscope was used. Through this analysis, spin-coated and brush coated film surface were compared. It was revealed that physical anisotropy was induced by brush coating at a high annealing temperature. Particles were aligned in one direction along which brush coating was made, resulting in a physical anisotropy that affects a uniform LC alignment. Therefore, it was confirmed that brush coating combined with BiAlO thin film annealed at high temperature has a significant potential for LC alignment.
In this study, the dielectric properties of flame retardant silicone rubber mixed with the amount of silica 50~65 phr were measured at frequencies ranging from 1 to 2.7 MHz and temperature ranges from 30℃ to 160℃. The permittivity decreased with higher frequencies and higher temperatures, and tanδ are thought to have decreased due to the increased heat oxidation of the methyl group bound to Si, which increased the hardness of silicone rubber. FT-IR analysis of specimen mixed with SiO2 of 50~65 phr showed oscillations of OH groups bound to SiO2 between wavenumber 3,600 and 3,300. As a result of analyzing surface components by Energy Dispersive X-ray (EDX) on all specimens mixed with SiO2 of 50 to 65 phr, all specimens contained Si, and the analysis by field emission scanning electron (FE-SEM) confirmed that about 1~5 μm particles were distributed regularly on the surface of the specimens.
Single-crystal diamond obtained by chemical vapor deposition (CVD) exhibits great potential for use in next-generation power devices. Low defect density is required for the use of such power devices in high-power operations; however, plastic deformation and lattice strain increase the dislocation density during diamond growth by CVD. Therefore, characterization of the dislocations in CVD diamond is essential to ensure the growth of high-quality diamond. In this work, we analyze the characteristics of the dislocations in CVD diamond through synchrotron white beam X-ray topography. In estimate, many threading edge dislocations and five mixed dislocations were identified over the whole surface.
In this work, in order to effectively improve the electrical conductivity and visible light transmittance of ZnO thin films, ZnO single layer and ZnO/Ag bi-layer films were deposited on glass substrates by radio frequency and direct current magnetron sputtering, and then, the effects of an Ag buffer layer and electron beam irradiation on the electrical and optical properties of the films were investigated. The observed results indicate that ZnO 100 nm / Ag 7 nm films show higher opto-electrical performance than the ZnO single layer film. In addition, electron beam irradiation also effectively enhanced the visible transmittance and electrical conductivity of the ZnO/Ag bi-layer films.
The perovskite solid solutions of the Sr1-xMgxFe3+ 1-τFe4+ τO3-y system (x=0.0, 0.1, 0.2, and 0.3) were synthesized in N2 at 1,150℃. X-ray powder diffraction study assured that all the four samples had cubic symmetries(SM-0: 3.865 Å, SM-1: 3.849 Å, SM-2: 3.833 Å, and SM-3: 3.820 Å) and that the lattice volumes decreased steadily from 57.7 Å3 to 55.7 Å3 with x values. The nonstoichiometric chemical formulas were determined by Mohr salt analysis and with the increase of x values the amounts of Fe4+ ion and oxygen were decreased simultaneously. Thermal analysis showed that SM-0 started to lose its oxygen at 450℃ and SM-1, Sm-2, and SM-3 began to lose their oxygen at around 350～400℃. SM-0 showed almost reversible weight change in the cooling process. All the samples exhibited semiconducting behaviors in the temperature range of 10~400℃. Conductivities of the 4 samples were decreased in the order of SM-0, SM-1, SM-2, and SM-3 at constant temperature. The activation energies of the conductions were in the range of 0.176 eV～0.244 eV.
This paper presents a study on the dispersion effect of the X-Ray diffraction, glass transition and DIMA properties of organic modifier clay/epoxy nanocomposites produced in a homogenizer. Several experiments were conducted including different types of dispersion condition with varying processing conditions such as homogenizer rotor speed and applied time of homogenizer. The effects of these variables on the dispersion properties of nanocomposites were then studied. In order to fully understand the experimental results, a X-ray diffraction, DSC and DMA were used to investigate the effect of above mentioned variables on microstructure and intercalation/exfoliation of organic modifier clay/epoxy nanocomposites. The results from this work could be used to determine the best processing condition to obtain appropriate levels of d-spacing, glasss transition temperature and storage modulus in organic modifier clay/epoxy nanocomposites.
AlN thin films were deposited on p-type Si(100) substrates by RF magnetron sputtering method. This study showed the change of the preferential orientation of AlN thin films deposition with the change of the deposition conditions such as sputtering pressure and Ar/N2 gas ratio in chamber. It was identified by X-ray diffraction patterns that AlN thin film deposited at low sputtering pressure has a (002) orientation, however its preferred orientation was changed from the (002) to the (100) orientation with increasing sputtering pressure. Also, it was observed that the properties of AlN thin films such as thickness, grain size and surface roughness were largely dependent on Ar/N2 gas ratio and a high quality thin film could be prepared at lower nitrogen concentration. AlN thin films were investigated relationship between preferential orientation and deposition condition by using XRD, FE-SEM and PFM.
In this study, a method to measure the thickness of thin film by EDS (energy dispersive spectroscopy) is suggested. We have developed a model which calculates the thickness of thin film from the characteristic x-ray intensity ratio of the elements in thin film and substrate by considering incident electron beam energy, x-ray generation curve, backscattering and absorption of x-ray, take-off angle of x-ray and tilt angle of the sample. We obtained the relation curve between the film thickness measured experimentally and the x-ray intensity ratio of elements. The film thicknesses calculated from the model agrees quite well with those measured experimentally. Therefore, the thin film thickness can be measured rapidly and accurately by using the model developed in this study and the x-ray intensity ratio obtained in EDS analysis.
Medical X-ray has been brought many changes according to the rapid development of high technology. Especially, for high-voltage generator which is the most important in X-ray generation the traditional way is to use high-voltage electric transformers primarily. However, since it is large and heavy and the ripple rate of DC high-voltage applied to X-ray tube is too big, it has a disadvantage of low X-ray production efficiency. To solve these problems, the studies about high-voltage power supply are now proceeding. At present, the high-voltage generator that generates high-voltage by making high frequency using inverter control circuit consisting of semiconductor device is mainly used. High-voltage generator using inverter has advantages in the diagnosis using X-ray including high performance with short-term use, miniaturization of power supply and ripple reduction. In this study, the X-ray high-voltage device with inverter type using pulse width modulation scheme to the control of tube voltage and tube current was designed and produced. For performance evaluation of produced device, the control signal analysis, irradiation dose change and beam quality depending on the load variation of tube voltage and tube current were evaluated.
In the study, the characteristics of the etched Zinc oxide (ZnO) thin films surface, the etch rate of ZnO thin film in Cl2/BCl3/Ar plasma was investigated. The maximum ZnO etch rate of 53 nm/min was obtained for Cl2/BCl3/Ar=3:16:4 sccm gas mixture. According to the x-ray diffraction (XRD) and atomic force microscopy (AFM), the etched ZnO thin film was investigated to the chemical reaction of the ZnO surface in Cl2/BCl3/Ar plasma. The field emission auger electron spectroscopy (FE-AES) analysis showed an elemental analysis from the etched surfaces. According to the etching time, the ZnO thin film of etched was obtained to The AES depth-profile analysis. We used to atomic force microscopy to determine the roughness of the surface. So, the root mean square of ZnO thin film was 17.02 in Cl2/BCl3/Ar plasma. Based on these data, the ion-assisted chemical reaction was proposed as the main etch mechanism for the plasmas.
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