• Title/Summary/Keyword: phase purity

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A topological metal at the surface of an ultrathin BiSb alloy film

  • Hirahara, T.;Sakamoto, Y.;Saisyu, Y.;Miyazaki, H.;Kimura, S.;Okuda, T.;Matsuda, I.;Murakami, S.;Hasegawa, S.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.14-15
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    • 2010
  • Recently there has been growing interest in topological insulators or the quantum spin Hall (QSH) phase, which are insulating materials with bulk band gaps but have metallic edge states that are formed topologically and robust against any non-magnetic impurity [1]. In a three-dimensional material, the two-dimensional surface states correspond to the edge states (topological metal) and their intriguing nature in terms of electronic and spin structures have been experimentally observed in bulk Bi1-xSbx single crystals [2,3,4]. However, if we want to know the transport properties of these topological metals, high purity samples as well as very low temperature will be needed because of the contribution from bulk states or impurity effects. In a recent report, it was also shown that an intriguing coupling between the surface and bulk states will occur [5]. A simple solution to this bothersome problem is to prepare a topological metal on an ultrathin film, in which the surface-to-bulk ratio is drastically increased. Therefore in the present study, we have investigated if there is a method to make an ultrathin Bi1-xSbx film on a semiconductor substrate. From reflection high-energy electron diffraction observation, it was found that single crystal Bi1-xSbx films (0${\sim}30\;{\AA}A$ can be prepared on Si(111)-$7{\times}7$. The transport properties of such films were characterized by in situ monolithic micro four-point probes [6]. The temperature dependence of the resistivity for the x=0.1 samples was insulating when the film thickness was $240\;{\AA}A$. However, it became metallic as the thickness was reduced down to $30\;{\AA}A$, indicating surface-state dominant electrical conduction. Figure 1 shows the Fermi surface of $40\;{\AA}A$ thick Bi0.92Sb0.08 (a) and Bi0.84Sb0.16 (b) films mapped by angle-resolved photoemission spectroscopy. The basic features of the electronic structure of these surface states were shown to be the same as those found on bulk surfaces, meaning that topological metals can be prepared at the surface of an ultrathin film. The details will be given in the presentation.

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Microstructure and Microdefects of Diamond Thin Films Deposited by MPECVD (마이크로웨이브 화학증착법에 의한 다이아몬드 박막의 미세구조오 미세결함)

  • Lee, Se-Hyeon;Lee, Yu-Gi;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.6 no.8
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    • pp.833-840
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    • 1996
  • Diamond thin films were deposited on p-type (100) Si wafers using MPECVD. Prior to deposition, ultrasonic striking was done to improve density of nucleation sites with dimond powder of 40~$60\mu$m size. Then diamond thin films were deposited at $^900{\circ}C$, 40Torr and 1000W microwave power using ${CH}_{4}$ and ${H}_{2}$ gases. The purity, the morphology and the microstructur'e and microdefects of diamond thin films were characterized by Raman spectroscopy, SEM and TEM, repectively. In Raman spectroscopy the peaks of non-diamond phase increased as ${CH}_{4}$, concentration increased. In SEM, the morphology of diamond thin films varied from crystalline to cauliflower as ${CH}_{4}$, concentration increased. As ${CH}_{4}$ con centration increased, the density of defects increased, with most defects being {III} twin. ${MTP}_{5}$, were formed with five (II]) planes. As these (Ill) Planes were twinned, ${MTP}_{5}$, represented five-fold symmetry. ]n the interfaces, defects in diamond thin films fanned out from small regions implying nucleation sites.

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Effect of Substrate Temperature and Growth Duration on Palladium Oxide Nanostructures (팔라듐 옥사이드 나노구조물의 성장에서 기판 온도와 성장 시간의 효과)

  • Kim, Jong-Il;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.458-463
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    • 2019
  • Palladium (Pd) is widely used as a catalyst and noxious gas sensing materials. Especially, various researches of Pd based hydrogen gas sensor have been studied due to the noble property, Pd can be adsorbed hydrogen up to 900 times its own volume. In this study, palladium oxide (PdO) nanostructures were grown on Si substrate ($SiO_2(300nm)/Si$) for 3 to 5 hours at $230^{\circ}C{\sim}440^{\circ}C$ using thermal chemical vapor deposition system. Pd powder (source material) was vaporized at $950^{\circ}C$ and high purity Ar gas (carrier gas) was flown with the 200 sccm. The surface morphology of as-grown PdO nanostructures were characterized by field-emission scanning electron microscopy(FE-SEM). The crystallographic properties were confirmed by Raman spectroscopy. As the results, the as-grown nanostructures exhibit PdO phase. The nano-cube structures of PdO were synthesized at specific substrate temperatures and specific growth duration. Especially, PdO nano-cube structrures were uniformly grown at $370^{\circ}C$ for growth duration of 5 hours. The PdO nano-cube structures are attributed to vapor-liquid-solid process. The nano-cube structures of PdO on graphene nanosheet can be applied to fabricate of high sensitivity hydrogen gas sensor.

A Study on the Leaching and Recovery of Lithium by Reaction between Ferric Chloride Etching Solution and Waste Lithium Iron Phosphate Cathode Powder (폐리튬인산철 양극재 분말과 염화철 에칭액과의 반응에 의한 리튬의 침출 및 회수에 대한 연구)

  • Hee-Seon Kim;Dae-Weon Kim;Byung-Man Chae;Sang-Woo Lee
    • Resources Recycling
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    • v.32 no.3
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    • pp.9-17
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    • 2023
  • Efforts are currently underway to develop a method for efficiently recovering lithium from the cathode material of waste lithium iron phosphate batteries (LFP). The successful application of lithium battery recycling can address the regional ubiquity and price volatility of lithium resources, while also mitigating the environmental impact associated with both waste battery material and lithium production processes. The isomorphic substitution leaching process was used to recover lithium from spent lithium iron phosphate batteries. Lithium was leached by the isomorphic substitution of Fe2+ in LFP using a relatively inexpensive ferric chloride etching solution as a leaching agent. In the study, the leaching rate of lithium was compared using the ferric chloride etching solution at various multiples of the LFP molar ratio: 0.7, 1.0, 1.3, and 1.6 times. The highest lithium leaching rate was shown at about 98% when using 1.3 times the LFP molar ratio. Subsequently, to eliminate Fe, the leachate was treated with NaOH. The Fe-free solution was then used to synthesize lithium carbonate, and the harvested powder was characterized and validated. The surface shape and crystal phase were analyzed using SEM and XRD analysis, and impurities and purity were confirmed using ICP analysis.

Automated Synthesis of [$^{18}F$]Fallypride for Routine Clinical Use (자동합성장치를 이용한 [$^{18}F$]Fallypride의 합성)

  • Park, Jun-Hyung;Moon, Byung-Seok;Lee, Hong-Jin;Lee, Hyo-Jun;Lee, In-Won;Lee, Byung-Chul;Kim, Sang-Eun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.14 no.2
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    • pp.104-109
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    • 2010
  • Purpose: $[^{18}F]$Fallypride plays an effective radiotracer for the study of dopamine $D_2/D_3$ receptor occupancy, neuropsychiatric disorders and aging in humans. This tracer has the potential for clinical use, but automated labeling efficiency showed low radiochemical yields about 5~20% with relatively long labelling time of fluorine-18. In present study, we describe an improved automatic synthesis of [$^{18}F$]Fallypride using different base concentration for routine clinical use. Materials and Methods: Fully automated synthetic process of [$^{18}F$]Fallypride was perform using the TracerLab $FX_{FN}$ synthesizer under various labeling conditions and tosyl-fallypride was used as a precursor. [$^{18}F$]Fluoride was extracted with various concentration of $K_{2.2.2.}/K_2CO_3$ from $^{18}O$-enriched water trapped on the ion exchange cartridge. After azeotropic drying, the labeling reaction proceeded in $CH_3CN$ at $100^{\circ}C$ for 10 or 30 min. The reaction mixture was purified by reverse phase HPLC and collected organic solution was exchanged by tc-18 Sep-Pak for the clinically available solution. Results: The optimal labeling condition of [$^{18}F$]Fallypride in the automatic production was that 2 mg of tosyl-fallypride in acetonitrile (1 mL) was incubated at $100^{\circ}C$ for 10 min with $K_{2.2.2.}/K_2CO_3$ (11/0.8 mg). [$^{18}F$]Fallypride was obtained with high radiochemical yield about $66{\pm}1.4%$ (decay-corrected, n=28) within $51{\pm}1.2$ min including HPLC purification and solid-phase purification for the final formulation. Conclusion: [$^{18}F$]Fallypride was prepared with a significantly improved radiochemical yield with high specific activity and shorten synthetic time. In addition, this automated procedure provides the high reproducibility with no synthesis failures (n=28).

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Corrosion Characteristics of Excavated Bronze Artifacts According to Corrosion Environment (부식 환경에 따른 출토 청동 유물의 부식 특성)

  • Jang, Junhyuk;Bae, Gowoon;Chung, Kwangyong
    • Korean Journal of Heritage: History & Science
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    • v.53 no.1
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    • pp.24-33
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    • 2020
  • In excavated bronze artifacts, corrosion products of various shapes and colors are observed due to multiple corrosion factors coexisting in the burial environment, and these corrosion products can constitute important data not only in terms of long-term corrosion-related information, but also in connection with preservation of artifacts. As such, scientific analysis is being carried out on the corrosion layer and corrosion products of bronze artifacts, and the corrosion mechanism and the characteristics of corrosion products elucidated, which is essential for interpreting the exposed burial environment and its association with corrosion factors inside the burial environment. In this study, after classifying excavated bronze artifacts according to alloy ratio and fabrication technique, comprehensive analysis of the surface of corrosion artifacts, corrosion layer, and corrosion products was carried out to investigate the corrosion mechanism, formation process of the corrosion layer, and characteristics of corrosion products. The study designated two groups according to alloy ratio and fabrication technique. In Group 1, which involved a Cu-Sn-Pb alloy and had no heat treatment, the surface was rough and external corrosion layers were formed on a part, or both sides, of the inside and the outside, and the surface was observed as being green or blue. α+δ phase selection corrosion was found in the metal and some were found to be concentrated in an empty space with a purity of 95 percent or more after α+δ phase corrosion. The Cu-Sn alloy and heat-treated Group 2 formed a smooth surface with no external corrosion layer, and a dark yellow surface was observed. In addition, no external corrosion layer was observed, unlike Group 1, and α corrosion was found inside the metal. In conclusion, it can be seen that the bronze artifacts excavated from the same site differ in various aspects, including the formation of the corrosion layer, the shape and color of the corrosion products, and the metal ion migration path, depending on the alloy ratio and fabrication technique. They also exhibited different corrosion characteristics in the same material, which means that different forms of corrosion can occur depending on the exposure environment in the burial setting. Therefore, even bronze artifacts excavated from the same site will have different corrosion characteristics depending on alloy ratio, fabrication technique, and exposure environment. The study shows one aspect of corrosion characteristics in specific areas and objects; further study of corrosion mechanisms in accordance with burial conditions will be required through analysis of the corrosive layer and corrosive product characteristics of bronze artifacts from various regions.

Physicochemical Characteristics of ${\beta}-Glucan$ Isolated from Barley (보리로부터 분리한 ${\beta}-Glucan$의 이화학적 특성)

  • Kim, Sung-Ran;Choi, Hee-Don;Seog, Ho-Moon;Kim, Sung-Soo;Lee, Young-Tack
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1164-1170
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    • 1999
  • The physicochemical characteristics of ${\beta}-glucan$ isolated from waxy and non-waxy barley were investigated. The hull-less waxy and non-waxy barley containing 6.5% and 5.3% of total ${\beta}-glucan$ respectively, were used as a starting material. The yield and ${\beta}-glucan$ content of crude ${\beta}-glucan$ from waxy barley was 5.54% and 62.9%, respectively, and those were higher than 3.34% and 59.2% from non-waxy barley. The crude ${\beta}-glucan$ purified with selective precipitation and enzymatic treatment to obtain the ${\beta}-glucan$ isolate of high purity (>99%). The total yield of purified ${\beta}-glucan$ from waxy and non-waxy barley was 4.46% and 2.59%, respectively. The surface appearance of the purified ${\beta}-glucan$ by scanning electron microscopy (SEM) showed randomly entangled multi-net structure of ${\beta}-glucan$ microfibrils. The melting temperature of ${\beta}-glucan$ from waxy and non-waxy barley measured by differential scanning calorimetry (DSC) was $184.6^{\circ}C$, and $180.3^{\circ}C$, respectively. DSC endotherm of ${\beta}-glucan$ solution showed 2 peaks near $68^{\circ}C$ and $84^{\circ}C$. Enthalpy of phase transition was higher in non-waxy ${\beta}-glucan$ than waxy ${\beta}-glucan$, and the intrinsic viscosity of ${\beta}-glucan$ solution from waxy barley was higher than that of non-waxy ${\beta}-glucan$. The pasting viscosity of barley starch with the purified ${\beta}-glucan$ determined by Rapid Visco-Analyzer was higher than that of barley starch without ${\beta}-glucan$, and the effect of ${\beta}-glucan$ on increasing the paste viscosity was greater in non-waxy barley starch.

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Study for the Synthesis of $[^{123}I]$Idoxifene and Its Uptake in the Breast Cancer Cell ($[^{123}I]$Idoxifene 합성과 유방암의 세포섭취에 관한 연구)

  • Cho, Young-Sub;Yang, Seung-Dae;Suh, Yong-Sup;Chun, Kwon-Soo;Ahn, Soon-Hyuk;Lim, Soo-Jung;Lim, Sang-Moo;Yu, Kook-Hyun
    • The Korean Journal of Nuclear Medicine
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    • v.34 no.5
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    • pp.410-417
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    • 2000
  • Purpose: Idoxifene is currently entering phase II clinical trials for the treatment of advanced breast cancer. The radiolabeled idoxifene using $[^{123}I]$ provides an opportunity for clinical pharmacology with single photon emission computed tomography (SPECT). The purpose of this study was to prepare radiolabeled idoxifene using $[^{123}I]$ and to determine its cell uptake of breast cancer cell line. Materials and Methods: With a view to evaluating new anticancer drugs, we are investigating the novel antiestrogen pyrrolidino-4-iodotamoxifen (idoxifene). $[^{123}I]$Idoxifene has been prepared in no-carrier-added form using a tributyl stannylated precursor which has been synthesized by means of (2-chloroethoxy)benzene with (${\pm}$)-2-phenylbutanoic acid on the basis of previously reported standard methods. The biodistribution and dynamic behavior of the compound were investigated using the comparative breast cancer cell line, MCF-7 (estrogen receptor-positive) and MDA-MB-468 (non-estrogen receptor). Results and Conclusion: Acylation of (2-chloroethoxy)benzene with (${\pm}$)-2-phenylbutanoic acid gave the versatile ketone (81%) which reacted with 1,4-diiodobenzene to give triphenylethylene as a mixture of E and Z geometric isomers, which were separated by the recrystallization in ethanol. The E-isomer was treated with pyrrolidine to give idoxifene (67%). In order to incorporate radioactive iodine into the 4-position, the 4-stannylated precursor was prepared (30%). The yield of radioiodination was 90-92% with a high radiochemical purity greater than 98%. The ratio of tumor uptake of the breast cancer cell line between MCF-7 and MDA-MB-468 was about 1.7.

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Radioimmunoassay for Determination of Serum Macrophage Migration Inhibitory Factor (혈중 대식세포 유주 저지 인자 측정을 위한 방사면역측정법)

  • Lee, Tae-Sup;Shin, Seok-Hwan;Song, Jee-In;Woo, Kwang-Sun;Chung, Wee-Sup;Choi, Chang-Woon;Lim, Sang-Moo
    • The Korean Journal of Nuclear Medicine
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    • v.38 no.6
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    • pp.532-539
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    • 2004
  • Purpose: There has been a renewal of interest in Macrophage migration inhibitory factor (MIF), especially correlation in pathogenesis of sepsis by many infectious diseases and in regulation of host inflammatory and immune response. We developed immunoradiometric assay (IRMA) to determine serum human MIF concentration. Materials and Methods: The IRMA system utilizes solid phase bound monoclonal anti-recombinant human MIF (rhMIF) antibody as a capture antibody, biotinylated polyclonal anti-rhMIF antibody as a detector antibody. We applied with rhMIF that concentration of standard solutions increased from 0 ng/ml to 100 ng/ml. We used $^{125}I$-streptavidin (SA) as radiotracer to determination of rhMIF concentration. Streptavidin was labeled with $^{125}I$ by Chloramine-T method and $^{125}I$-SA was purified by ultracentrifugation. $^{125}I$-SA stability was evaluated by ITLC analysis at $4^{\circ}C$ and room temperatures until 60days. To validate IRMA system for MIF, we experimented intra-assay and inter-assay coefficients of variation, recovery test and dilution test. Results: Radiolabeling yield of $^{125}I$-SA was 87% and purified $^{125}I$-SA retained above 99% radiochemical purity. $^{125}I$-SA showed above 93% stability in $4^{\circ}C$ until 60days that it is good for immunoradiometric assay as radiotracer. Plotted standard dose response curve showed that increased concentration of rhMIF linearly correlated (R2=0.99) with bound radioactivity of $^{125}I$-SA. The highest intra- and inter-assay coefficients of variation were 5.5% and 7.6%, respectively. The average of recovery of MIF in samples was 102%. In dilution test, linear response curves were obtained (R2=0.97). Conclusion: Radioimmunoassay using $^{125}I$-SA as radiotracer thought to be useful for the determination of serum MIF concentration, and further, its data will be used to evaluate the correlation between clinical significance and serum MIF concentration in patients with various inflammatory diseases.

Synthesis of a Dopamine Transporter Imaging Agent, N-(3-[$^{18}F$]fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane (도파민운반체 방사성추적자 N-(3-[$^{18}F$Fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane의 합성)

  • Choe, Yearn-Seong;Oh, Seung-Jun;Chi, Dae-Yoon;Kim, Sang-Eun;Choi, Yong;Lee, Kyung-Han;Kim, Byung-Tae
    • The Korean Journal of Nuclear Medicine
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    • v.33 no.3
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    • pp.298-305
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    • 1999
  • Purpose: N-(3-[$^{18}F$]Fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane [$^{18}F$]FP-CIT) has been shown to be very useful for imaging the dopamine transporter. However, synthesis of this radiotracer is somewhat troublesome. In this study, we used a new method for the preparation of [$^{18}F$]FP-CIT to increase radiochemical yield and effective specific activity. Materials and Methods: [$^{18}F$]FP-CIT was prepared by N-alkylation of nor-${\beta}$-CIT (2 mg) with 3-bromo-1-[$^{18}F$]fluoropropane in the presence of $Et_3N$ (5-6 drops of $DMF/CH_3CN$, $140^{\circ}C$, 20 min). 3-Bromo-1-[$^{18}F$]fluoropropane was synthesized from $5{\mu}L$ of 3-bromo-1-trifluoromethanesulfonyloxypropane (3-bromopropyl-1-triflate) and $nBu_4N^{18}F$ at $80^{\circ}C$. The final compound was purified by reverse phase HPLC and formulated in 13% ethanol in saline. Results: 3-Bromo-1-[$^{18}F$]fluoropropane was obtained from 3-bromopropyl-1-triflate and $nBu_4N^{18}F$ in 77-80% yield. N-Alkylation of nor-${\beta}$-CIT with 3-bromo-1-[$^{18}F$]fluoropropane was carried out at $140^{\circ}C$ using acetonitrile containing a small volume of DMF as the solvents. The overall yield of [$^{18}F$]FP-CIT was 5-10% (decay-corrected) with a radiochemical purity higher than 99% and effective specific activity higher than the one reported in the literature based on their HPLC data. The final [$^{18}F$]FP-CIT solution had the optimal pH (7.0) and it was pyrogen-free. Conclusion: In this study, 3-bromopropyl-1-triflate was used as the precursor for the [$^{18}F$]fluorination reaction and new conditions were developed for purification of [$^{18}F$]FP-CIT by HPLC. We established this new method for the preparation of [$^{18}F$]FP-CIT, which gave high effective specific activity and relatively good yield.

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