• Polymer(Korea)
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• v.29 no.1
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• pp.87-90
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• 2005

In this study, we have examined the exfoliation behavior of layered clay during in-situ polymeriztion with styrene by using real-time XRD analysis. The 4C1 beam line at the Pohang Accelerator Laboratory (PAL) was used for this study. Different exfoliation behaviors have been shown to depend on the cation exchange capacity (CEC) of clay and the chemical structure of organic modifiers. For 10A-MMT and 15A-MMT having high CEC, no peak shifts were observed on real-time XRD analysis during polymerization. However, 2$\theta$ for 25A-MMT and VDAC-MMT, each having low CEC’s as well as aromatic benzene moieties and vinyl groups, respectively, decreased as polymerization time increased.

• Nuclear Engineering and Technology
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• v.56 no.2
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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.

• Korean Journal of Metals and Materials
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• v.49 no.1
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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.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.32 no.1
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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.

• Particle and aerosol research
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• v.17 no.1
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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.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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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.

• Economic and Environmental Geology
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• v.51 no.4
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• pp.359-370
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• 2018

The batch and column experiments were performed to overcome the limitation of the neutralization process using the $scCO_2$-water-recycled aggregate, reducing its treatment time to 3 hour. The waste cement mortar and two kinds of recycled aggregate were used for the experiment. In the extraction batch experiment, three different types of waste mortar were reacted with water and $scCO_2$ for 1 ~ 24 hour and the pH of extracted solution from the treated waste mortar was measured to determine the minimum reaction time maintaining below 9.8 of pH. The continuous column experiment was also performed to identify the pH reduction effect of the neutralization process for the massive recycled aggregate, considering the non-equilibrium reaction in the field. Thirty five gram of waste mortar was mixed with 70 mL of distilled water in a high pressurized stainless steel cell at 100 bar and $50^{\circ}C$ for 1 ~ 24 hour as the neutralization process. The dried waste mortar was mixed with water at 150 rpm for 10 min. and the pH of water was measured for 15 days. The XRD and TG/DTA analyses for the waste mortar before and after the reaction were performed to identify the mineralogical change during the neutralization process. The acryl column (16 cm in diameter, 1 m in length) was packed with 3 hour treated (or untreated) recycled aggregate and 220 liter of distilled water was flushed down into the column. The pH and $Ca^{2+}$ concentration of the effluent from the column were measured at the certain time interval. The pH of extracted water from 3 hour treated waste mortar (10 ~ 13 mm in diameter) maintained below 9.8 (the legal limit). From XRD and TG/DTA analyses, the amount of portlandite in the waste mortar decreased after the neutralization process but the calcite was created as the secondary mineral. From the column experiment, the pH of the effluent from the column packed with 3 hour treated recycled aggregate kept below 9.8 regardless of their sizes, identifying that the recycled aggregate with 3 hour $scCO_2$ treatment can be reused in real construction sites.

• Advances in nano research
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• v.13 no.6
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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.

• Economic and Environmental Geology
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• v.50 no.4
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• pp.257-266
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• 2017

Batch experiments were performed to develop the method for the pH reduction of recycled aggregate by using $scCO_2$ (supercritical $CO_2$), maintaining the pH of extraction water below 9.8. Three different aggregate types from a domestic company were used for the $scCO_2$-water-recycled aggregate reaction to investigate the low pH maintenance of aggregate during the reaction. Thirty five gram of recycled aggregate sample was mixed with 70 mL of distilled water in a Teflon beaker, which was fixed in a high pressurized stainless steel cell (150 mL of capacity). The inside of the cell was pressurized to 100 bar and each cell was located in an oven at $50^{\circ}C$ for 50 days and the pH and ion concentrations of water in the cell were measured at a different reaction time interval. The XRD and SEM-EDS analyses for the aggregate before and after the reaction were performed to identify the mineralogical change during the reaction. The extraction experiment for the aggregate was also conducted to investigate the pH change of extracted water by the $scCO_2$ treatment. The pH of the recycled aggregate without the $scCO_2$ treatment maintained over 12, but its pH dramatically decreased to below 7 after 1 hour reaction and maintained below 8 for 50 day reaction. Concentration of $Ca^{2+}$, $Si^{4+}$, $Mg^{2+}$ and $Na^+$ increased in water due to the $scCO_2$-water-recycled aggregate reaction and lots of secondary precipitates such as calcite, amorphous silicate, and hydroxide minerals were found by XRD and SEM-EDS analyses. The pH of extracted water from the recycled aggregates without the $scCO_2$ treatment maintained over 12, but the pH of extracted water with the $scCO_2$ treatment kept below 9 of pH for both of 50 day and 1 day treatment, suggesting that the recycled aggregate with the $scCO_2$ treatment can be reused in real construction sites.