• Title/Summary/Keyword: XRD Diffraction

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A Study on the Reaction of Al-1% Si with Ti-silicide (Al-1% Si층과 Ti-silicide층의 반응에 관한 연구)

  • Hwang, Yoo-Sang;Paek, Su-Hyon;Song, Young-Sik;Cho, Hyun-Choon;Choi, Jin-Seog;Jung, Jae-Kyoung;Kim, Young-Nam;Sim, Tae-Un;Lee, Jong-Gil;Lee, Sang-In
    • Korean Journal of Materials Research
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    • v.2 no.6
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    • pp.408-416
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    • 1992
  • Stable TiS$i_2$was formed by RTA on single-Si and on poly-Si. Subsequently, an Al-1% Si layer with 600-nm thick was deposited on top of the TiS$i_2$, Finally, the specimens were annealed for 30min at 400-60$0^{\circ}C$in $N_2$ambient. The thermal stability of Al-1% Si/TiS$i_2$bilayer and interfacial reaction were investigated by measuring sheet resistance, Auger electron spectroscopy (AES), and scanning electron microscopy (SEM). The composition and phase of precipitates formed by the reaction of Al-1% Si with Ti-silicide were studied by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD). In the case of single-Si substrate the reaction of Al-1% Si layer with TiS$i_2$layer resulted in precipitates, consuming all TiS$i_2$layer at 55$0^{\circ}C$. On the other hand, the disappearance of TiS$i_2$on poly-Si occurred at 50$0^{\circ}C$ and more precipitates were formed by the reaction of Al-1% Si/TiS$i_2$on potty-Si substrate than those of the reaction on single-Si substrate. This phenomenon resulted from the fact that Ti-silicide formed on poly-Si was more unstable than on single-Si by the effect of grain boundary. By EDS analysis the precipitates were found tobe composed of Ti, Al, and Si. X-ray diffraction showed the phase of precipitates to be theT$i_7$A$l_5$S$i_12$ternary compound.

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Revealing the Paleo-ocean Environment of OSM-XX in the Western Pacific Magellan Seamount with Mineralogical and Geochemical Properties of Ferromanganese Crust (서태평양 마젤란해산군 OSM-XX 해저산 망간각의 광물학적, 지화학적 특성과 고해양 고환경 복원 연구)

  • Jinsub Park;Kiho Yang
    • Economic and Environmental Geology
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    • v.56 no.1
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    • pp.55-63
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    • 2023
  • Variations in geochemical and mineralogical properties of the ferromanganese(Fe-Mn) crust reflect environmental changes. In the present study, geochemical and mineralogical analyses, including micro X-ray fluorescence and X-ray diffraction, were utilized to reconstruct the paleo-ocean environment of western Pacific Magellan seamount cluster. Samples of the Fe-Mn crust were collected using an epibenthic sledge from the open seamount XX (151° 51.12' 7.2" E and 16° 8.16' 9.6" N, 1557 meters below sea level) in the Western Pacific Magellan Seamount. According to the structure and phosphating status, the Fe-Mn crust of the OSM-XX can be divided into the following: phosphatizated (L4-L5), massive non-phosphatizated (L3), and porous non-phosphatizated (L1-L2) portions. All ferromanganese layers contain vernadite, and owing to the presence of carbonate fluorapatite (CFA), the phosphatizated portion (L4-L5) is rich in Ca and P. The massive non-phosphatizated section (L3) contains high Mn, Ni, and Co, whereas the porous non-phosphatizated portion (L1-L2), which comprises detrital quartz and feldspar, is rich in Fe. Variations in properties of the Fe-Mn crust from the OSM-XX reflect changes in the nearby marine environment. The formation of this crust started at approximately 51.87 Ma, and precipitation of the CFA during the global phosphatization event that occurred at approximately 36-32 Ma highlights an elevated sea level and low temperature during the associated period. The high Mn, Ni, and Co concentrations and elevated Mn/Fe ratios of samples from the massive phosphatizated portion indicate that the oxygen minimum zone (OMZ) was enhanced, and reducing conditions prevailed during the crust formation. The high Fe and low Mn/Fe ratios in the porous portion indicate a weak OMZ and dominantly oxidizing conditions. These data reflect environmental changes following the end of the Mi-1 glacial period in the Miocene-Oligocene boundary. Subsequently, Mn/Fe and Co/Mn ratios increased slightly in the outermost part of Fe-Mn crust because of the enhanced bottom current and OMZ associated with the continued cooling from approximately 9 Ma. However, the reduced carbonate dissolution rate in the Pacific Ocean from approximately 6 Ma decreased the growth rate of the Fe-Mn crust.

Heat Shield Property of Nanostructural-regulated Fe2O3/TiO2 Composites Filled with Polyacrylate Paint (나노구조 변화에 의한 Fe2O3/TiO2 복합재료를 충전한 Poly Acrylate 도료의 열차단 특성)

  • Kim, Dae Won;Ma, Young Kil;Kim, Jong Seok
    • Applied Chemistry for Engineering
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    • v.31 no.1
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    • pp.43-48
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    • 2020
  • Fe2O3 nanoparticles with the mixed structure of cubic and nanorod were synthesized by precipitation, hydrothermal, sol-gel method, etching process and heat treatment. Fe2O3/TiO2 core-shell (CS) of type Fe2O3@TiO2 composite was fabricated on a 20 nm nanolayer of TiO2 coated on the surface of Fe2O3 nanoparticles. Fe2O3/TiO2 yolk-shell (YS) composite was prepared by chemical etching and heat treatment of Fe2O3/TiO2 CS nanoparticles. Physical properties of Fe2O3, Fe2O3@TiO2 CS and Fe2O3@TiO2 YS nanoparticles were characterized by FE-SEM, HR-TEM and X-ray diffraction. The solar reflectance, commission internationale de l'Elcairage (CIE) color coordinate and heat shield temperatures of Fe2O3, CS and YS type Fe2O3@TiO2 pigments filled with poly acrylate (PA) paints were investigated by UV-Vis-NIR spectrometer and homemade heat shield temperature measuring device. The Fe2O3@TiO2 YS red pigment filled PA composite exhibited excellent near infrared light reflecting performance and also reduced the heat shield temperature of 13 ℃ than that of Fe2O3 filled counterparts.

Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1) (Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구)

  • Park, Il-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.18 no.2
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) fabricated by sol-gel and vacuum sealed annealing process. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) have been studied by x-ray diffraction(XRD), vibrating sample magnetometer, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures were found to be a cubic garnet structure with space group Ia3d. The determined lattice constants $a_0$ of x = 0, and 1 are $12.497\AA$, and $12.465\AA$, respectively. The distribution of gallium and iron in $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ is studied by Rietveld refinement. Based on Rietveld refinement results, the terbium and bismuth ions occupy the 24c site, iron ions occupy the 24d, l6a site, and nonmagmetic gallium ions occupy the 16a site. In order to verify the magnetic site occupancy of iron and gallium, we have taken $M\ddot{o}ssbauer$ spectra for $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) at room temperature. From the results of $M\ddot{o}ssbauer$ spectra analysis, the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 60.8 % and 39.2 %, respectively, and the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 74.7 % and 25.3 %, respectively. It is noticeable that all of the nonmagnetic Ga atoms occupy the 16a site by vacuum annealing process.

Improved Electrochemical Performance and Minimized Residual Li on LiNi0.6Co0.2Mn0.2O2 Active Material Using KCl (KCl을 사용한 LiNi0.6Co0.2Mn0.2O2계 양극활물질의 잔류리튬 저감 및 전기화학특성 개선)

  • Yoo, Gi-Won;Shin, Mi-Ra;Shin, Tae-Myung;Hong, Tae-Whan;Kim, Hong-kyeong
    • Journal of the Korean Electrochemical Society
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    • v.20 no.1
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    • pp.7-12
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    • 2017
  • Using a precursor of $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ as a starting material, a surface-modified cathode material was obtained by coating with KCl, where the added KCl reduces residual Li compounds such as $Li_2CO_3$ and LiOH, on the surface. The resulting electrochemical properties were investigated. The amounts of $Li_2CO_3$ and LiOH decreased from 8,464 ppm to 1,639 ppm and from 8,088 ppm to 6,287 ppm, respectively, with 1 wt% KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ that had been calcined at $800^{\circ}C$. X-ray diffraction results revealed that 1 wt% of KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ did not affect the parent structure but enhanced the development of hexagonal crystallites. Additionally, the charge transfer resistance ($R_{ct}$) decreased dramatically from $225{\Omega}$ to $99{\Omega}$, and the discharge capacity increased to 182.73mAh/g. Using atomic force microscopy, we observed that the surface area decreased by half because of the exothermic heat released by the Li residues. The reduced surface area protects the cathode material from reacting with the electrolyte and hinders the development of a solid electrolyte interphase (SEI) film on the surface of the oxide particles. Finally, we found that the introduction of KCl into $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ is a very effective method of enhancing the electrochemical properties of this active material by reducing the residual Li. To the best of our knowledge, this report is the first to demonstrate this phenomenon.

Pedological and Mineralogical Characterizations of Hwangto (Yellow Residual Soils), Naju, Jeollanam-do, Korea (전라남도 나주시 동강면 일대 황토(풍화잔류토)의 토양학적 및 광물학적 특성 연구)

  • Kim, Yumi;Bae, Jo-Ri;Kim, Cheong-Bin;Roh, Yul
    • Economic and Environmental Geology
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    • v.47 no.2
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    • pp.87-96
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    • 2014
  • The objectives of this study were to characterize the physicochemical properties and mineralogy of Hwangto (yellow residual soils) from the southwestern part of Korea and to understand the soil-forming processes of the residual soils from their parent rocks. Both the yellowish residual soils as well as the unweathered and weathered parent rocks were obtained from Jangdong-ri, Donggang-myun, Naju, Jeollanam-do, Korea. The soil samples were examined to analyze the said soil's physicochemical properties such as color, pH, and particle size distribution. A scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis were performed in order to understand the mineralogy, chemical composition, and morphology of the soils. Two thin sections of a parent rock were analyzed to study its mineral composition. A particle size analysis of the soils indicates that the residual soil consists of mainly silt and clay (approximately 95%) and that soil textures are silty clay or silt clay loam. The soil colors of the residual soil are dark brown (7.5YR 3/4) through yellowish red (5YR 4/6). The pH of the residual soil ranges from 4.3 to 5.1. The major minerals of the parent rocks were quartz, biotite, chlorite, and plagioclase. The mineralogy of the sand fraction of the residual soil was quartz, biotite, muscovite and sanidine. The mineralogy of the silt fraction of the residual soil was quartz, biotite, muscovite, Na-feldspar, K-feldspar, and sanidine. The clay mineralogy of the soil was goethite, kaolinite, ilite, hydroxy-interlayed vermiculite(HIV), vermiculite, mica, K-feldspar and quartz. The mineral composition of the residual soil and the parent rock indicates that feldspar and mica in the parent rock weathered into illite, vermiculite and hydroxy-interlayed vermiculite(HIV), and finally changed into kaolinite and halloysite in the yellowish residual soils.

Synthesis and Screening of the System $SrO-Gd_2O_3-Al_2O_3$Doped with Tb by Polymerized-Complex Combinatorial Chemistry (고분자 착체 조합 화학법을 이용한 Tb이 첨가된 $SrO-Gd_2O_3-Al_2O_3$계 형광물질의 합성 및 탐색)

  • Jeong, Yang Sun;Kim, Chang Hae;Park, Hee Dong;Park, Joon Taik;Kang, Sung Kwon
    • Journal of the Korean Chemical Society
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    • v.45 no.5
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    • pp.461-469
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    • 2001
  • The combinatorial approach has been applied to discover and optimize the composition of the novel or enhanced materials. In this study, we screened the optimum composition of the system SrO-Gd$_2$O$_3$-Al$_2$O$_3$ doped with $Tb^{3+}$ by a polymerized-complex combinatorial chemistry method. Mixtures with compositions of Sr, Gd and Al component that is in the range from 0 to 1 in about 0.05 increments could be tested. The sample powders were synthesized by a polymerized complex method. To prepare appropriately polymeric precursors, we used the metallic nitrates, citric acid and ethylene glycol. The luminescence properties of the synthesized powders are investigated using the UV and VUV (Vacuum-UV: 147 nm) photoluminescence spectrometer. In addition, the crystallinity and morphology of powder were monitored by X-ray diffraction spectrometer and scanning electron microscopy. In result of VUV PL works, there are good luminescent samples with the composition of 0.595 < x < 0.733 and 0.016 < y < 0.017 in Gd1-x-yAlxTbyO$\delta$ and 0.049 < x < 0.064 and 0.02 < y < 0.039 in $Sr_xAl_{1-x-y}Tb_yO_$\delta$$, their materials can be applicable to plasma display panels as the green phosphor.

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Mineralogical, Micro-textural, and Geochemical Characteristics for the Carbonate Rocks of the Lower Makgol Formation in Seokgaejae Section (석개재 지역 하부 막골층 탄산염암의 광물조성, 미세구조 및 지화학적 특성)

  • Park, Chaewon;Kim, Ha;Song, Yungoo
    • Economic and Environmental Geology
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    • v.51 no.4
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    • pp.323-343
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    • 2018
  • This study defines the mineralogical, micro-textural and geochemical characteristics for the carbonate rocks and discusses the fluids that have affected the depositional environment of the Lower Makgol Formation in Seokgaejae section. Based on analysis of X-ray Diffraction (XRD), Scanning Electron Microscope-Energy Dispersive X-ray Spectrometry (SEM-EDS), Electron Probe Micro Analyzer-Wavelength Dispersive X-ray Spectrometry (EPMA-WDS) and Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS), carbonate miorofacies in the basal and the lower members of the Makgol Formation are distinguished and classified into four types. Type 1 dolomite (xenotopic interlocking texture) and Type 2 dolomite (idiotopic interlocking texture) have relatively high Mg/Ca ratio, flat REE pattern, low Fe and Mn. Extensively interlocking textures in these dolomites indicate constant supply of Mg ion from hypersaline brine. Type 3 and Type 4 dolomite (scattered and loosely-aggregated texture) have relatively moderate Mg/Ca ratio, MREE enriched pattern, low to high Fe and Mn. These partial dolomitization indicate limited supply of Mg ion under the influx of meteoric water with seawater. Also, the evidence of Fe-bearing minerals, recrystallization and relatively high Fe and Mn in Type 4 indicates the influence of secondary diagenetic fluids under suboxic conditions. Integrating geochemical data with mineralogical and micro-textural evidence, the discrepancy between the basal and the lower members of the Makgol Formation indicates different sedimentary environment. It suggest that hypersaline brine have an influence on the basal member, while mixing meteoric water with seawater have an effect on the lower member of the Makgol Formation.

Effects of Magnesium on Sulfate Resistance of Alkali-activated Materials (알칼리 활성화 결합재의 황산염 침식에 미치는 마그네슘의 영향)

  • Park, Kwang-Min;Cho, Young-Keun;Ra, Jung-Min;Kim, Hyung-Suk
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.21 no.1
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    • pp.109-116
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    • 2017
  • This paper describes the investigation into the durability alkali-activated materials(AAM) mortar and paste samples manufactured using fly-ash(FA) and ground granulated blast furnace slag(GGBFS) exposed to a sulfate environment with different GGBFS replace ratios(30, 50 and 100%), sodium silicate modules($Ms[SiO_2/Na_2O]$ 1.0, 1.5 and 2.0). The tests involved immersions into 10% sodium sulfate solution($Na_2SO_4$), 10% magnesium sulfate solution($MgSO_4$), 10% magnesium nitrate solution($Mg(NO_3)_2$) and 5% magnesium nitrate($Mg(NO_3)_2$+5% sodium sulfate solution+$Na_2SO_4$). The evolution of compressive strength, weight, length expansion and microstructural observation such as x-ray diffraction were studied. As a results, in case of immersed in $Na_2SO_4$, $Mg(NO_3)_2$ and $Mg(NO_3)_2+Na_2SO_4$ shows increase in long-term strength. However, for samples immersed in $MgSO_4$, the general observation was that the compressive strength decreased after immersion. The most drastic reduction of compressive strength and expansion of weight and length occurred when GGBFS or Ms ratios were higher. Also, the XRD analysis of samples immersed in magnesium sulfate indicated that expansion of AAM caused by gypsum($CaSO_4{\cdot}2H_2O$) and brucite(MgOH). The results showed that, an additional condition $Mg^{2+}$ in which ${SO_4}^{2-}$ is the presence of a certain concentration, sulfate erosion has to be accelerated.

Preparation and Reactivity of Cu-Zn-Al Based Hybrid Catalysts for Direct Synthesis of Dimethyl Ether by Physical Mixing and Precipitation Methods (물리혼합 및 침전법에 의한 DME 직접 합성용 Cu-Zn-Al계 혼성촉매의 제조 및 반응특성)

  • Bang, Byoung Man;Park, No-Kuk;Han, Gi Bo;Yoon, Suk Hoon;Lee, Tae Jin
    • Korean Chemical Engineering Research
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    • v.45 no.6
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    • pp.566-572
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    • 2007
  • Two hybrid catalysts for the direct synthesis of DME were prepared and the catalytic activity of these catalysts were investigated. The hybrid catalyst for the direct synthesis of DME was composed as the catalytic active components of methanol synthesis and dehydration. The methanol synthesis catalyst was formed from the precursor contained Cu and Zn, the methanol dehydration catalyst was used ${\gamma}-Al_2O_3$. As PM-CZ+D and CP-CZA/D, Two hybrid catalysts were prepared by physical mixing method (PM-CZ+D) and precipitation method (CP-CZA/D), respectively. PM-CZ+D was prepared by physically mixing methanol synthesis catalyst and methanol dehydration catalyst, CP-CZA/D was prepared by depositing Cu-Zn or Cu-Zn-Al components on ${\gamma}-Al_2O_3$. The crystallinity and the surface morphology of synthesized catalyst were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) to investigate the physical property of prepared catalyst. And BET surface area by $N_2$ adsorption and the surface area of Cu by $N_2O$ chemisorption were investigated about the hybrid catalysts. In addition, catalytic activity of these hybrid catalysts was examined with varying reaction conditions. At that time, the reaction temperature of $250{\sim}290^{\circ}C$, the reaction pressure of 50~70 atm, the $[H_2]/[CO]$ mole ratio of 0.5~2.0 and the space velocity of $1,500{\sim}6,000h^{-1}$ were investigated the catalytic activity. From these results, it was confirmed that the reactivity of CP-CZA/D was higher than that of PM-CZ+D. When the conditions of reaction temperature, pressure, $[H_2]/[CO]$ ratio and space velocity were $260^{\circ}C$, 50 atm and 1.0, $3,000h^{-1}$ respectively, CO conversion using CP-CZA/D hybrid catalyst was 72% and the CO conversion of CP-CZA/D was more than 20% compared with the CO conversion of PM-CZ+D. It was known that Cu surface area of CP-CZA/D hybrid catalyst was higher than that of hybrid PM-CZ+D catalyst using $N_2O$ chemisorption. It was assumed that the catalytic activity was improved because Cu particle of hybrid catalyst prepared by precipitation method was well dispersed.