• Title/Summary/Keyword: 정량 XRD 분석

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Study on Ti-doped LiNi0.6Co0.2Mn0.2O2 Cathode Materials for High Stability Lithium Ion Batteries (고안정성 리튬이온전지 양극활물질용 Ti 치환형 LiNi0.6Co0.2Mn0.2O2 연구)

  • Jeon, Young Hee;Lim, Soo A
    • Journal of the Korean Electrochemical Society
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    • v.24 no.4
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    • pp.120-132
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    • 2021
  • Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO2, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi0.6Co0.2Mn0.2O2, precursor Ni0.6Co0.2Mn0.2-x(OH)2/xTiO2 was prepared using a nanosized TiO2 suspension type source for uniform Ti substitution in the precursor. It was mixed with Li2CO3, and after heating, the cathode active material LiNi0.6Co0.2Mn0.2-xTixO2 was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.

Synthesis of Garnet in the Ca-Ce-Gd-Zr-Fe-O System (Ca-Gd-Ce-Zr-Fe-O계에서의 석류석 합성 연구)

  • Chae Soo-Chun;Jang Young-Nam;Bae In-Kook;Yudintsev S.V.
    • Economic and Environmental Geology
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    • v.38 no.2 s.171
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    • pp.187-196
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    • 2005
  • Structural sites which cations can occupy in garnet structure are centers of the tetrahedron, octahedron, and distorted cube sharing edges with the tetrahedron and octahedron. Among them, the size of cation occuping at tetrahedral site (the center of tetrahedron) is closely related with the size of a unit cell of garnet. Accordingly, garnet containing iron with relative large ionic radii in tetrahedral site can be considered as a promising matrix for the immobilization of the elements with large ionic radii, such as actinides in radioactive wastes. We synthesized several garnets with the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$, and studied their properties and phase relations under various conditions. Mixed samples were fabricated in a pellet form under a pressure of $200{\~}400{\cal}kg/{\cal}cm^2$ and were sintered in the temperature range of $1100\~1400^{\circ}C$ in air and under oxygen atmospheres. Phase identification and chemical analysis of synthesized samples were conducted by XRD and SEM/EDS. In results, garnet was obtained as the main phase at $1300^{\circ}C$, an optimum condition in this system, even though some minor phases like perovskite and unknown phase were included. The compositions of garnet and perovskite synthesized from the batch composition of $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$ were ranged $[Ca_{l.2-1.8}Gd_{0.9-1.4}Ce_{0.3-0.5}]^{VIII}[Zr_{0.8-1.3}Fe_{0.7-1.2}]^{VI}[Fe_{2.9-3.1}]^{IV}O_{12}$ and $Ca_{0.1-0.5}Gd_{0.0-0.8}Ce_{0.1-0.5}\;Zr_{0.0-0.2}Fe_{0.9-1.1}O_3$, respectively. Ca content was exceeded and Ce content was depleted in the 8-coordinated site, comparing to the initial batch composition. This phenomena was closely related to the content of Zr and Fe in the 6-coordinated site.

Formation of the $CoSi_{2}$ using Co/Zr Bilayer on the Amorphous and the Single Crystalline Si Substrates (단결정과 비정질 Si 기판에서 Co/Zr 이중층을 이용한 $CoSi_{2}$ 형성)

  • Kim, Dong-Wook;Jeon, Hyeong-Tag
    • Korean Journal of Materials Research
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    • v.8 no.7
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    • pp.621-627
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    • 1998
  • The formation of Co-silicide between Co/Zr bilayer on the amorphous and crystalline Si substrates has been investigated. The films of Zr(50$\AA$) and Co(l50$\AA$) were deposited with e-beam evaporation system and were heattreated with the rapid thermal annealing system at the temperatures between 50$0^{\circ}C$ and 80$0^{\circ}C$ with 10$0^{\circ}C$ increments for 30 seconds. The phase identification of Co-silicide was carried out by XRD and the chemical analysis was examined by AES and RBS. The interface morphologies of Co/Zr bilayer films were investigated by cross sectional TEM and HRTEM. $CoSi_2$ was formed epitaxially on the crystalline Si substrate above $700^{\circ}C$ while polycrystalline $CoSi_2$ was grown on the amorphous Si substrate. The formation temperature of Co-silicide on the amorphous Si substrate was about 100 C lower than that on the crystalline Si. The COzSi phase was not identified on the both Si substrates. The formation temperature of first phase of Co-silicide on ColZr bilayer was higher than that on Co mono layer. CoSizlayer formed on the amorphous Si substrate exhibits better uniformity compared to the CoSiz formed on the crystalline substrate. The sheet resistance of CoSiz layer on crystalline Si was lower than that on the amorphous Si at high temperatures.tures.

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Synthesis of Fe­Garnet for tile Immobilization of High Level Radioactive Waste (고준위 방사성폐기물의 고정화를 위한 Fe­석류석 합성 연구)

  • ;;;Yudintsev, S. V.
    • Journal of the Mineralogical Society of Korea
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    • v.16 no.4
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    • pp.307-320
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    • 2003
  • Garnet has been considered as a possible matrix for the immobilization of radioactive actinides. It is expected that Fe­based garnet be able to have the high substitution ability of actinide elements because ionic radius of Fe in tetrahedral site is larger than that of Si of Si­based garnet. Accordingly, we synthesized Fe­garnet with the batch composition of $Ca_{2,5}$C $e_{0.5}$Z $r_2$F $e_3$ $O_{12}$ and $Ca_2$CeZrFeF $e_3$ $O_{12}$ and studied their phase relations and properties. Mixed samples were fabricated in pellet forms under the pressure of 400 kg/$\textrm{cm}^2$ and were sintered in the temperature range of 1100∼140$0^{\circ}C$ in atmospheric conditions. Phase identification and chemical composition of synthesized samples were analyzed by XRD and SEM/EDS. In results, where the compounds were sintered at 130$0^{\circ}C$, we optimally obtained Fe­garnets as the main phase, even though some minor phases like perovskite were included. The compositions of Fe­garnets synthesized from the batch compositions of $Ca_{2,5}$C $e_{0.5}$Z $r_2$F $e_3$ $O_{12}$ and $Ca_2$CeZrFeF $e_3$ $O_{12}$, are $Ca_{2.5­3.2}$C $e_{0.3­0.7}$Z $r_{1.8­2.8}$F $e_{1.9­3.2}$ $O_{12}$ and $Ca_{2.2­2.5}$C $e_{0.8­1.0}$Z $r_{1.3­1.6}$ F $e_{0.4­.07}$ F $e_{3­3.2}$ $O_{12}$, respectively. Ca contents were exceeded and Ce contents were exceeded or depleted in 8­coodinated site, comparing to the initial batch composition. These results were caused by the compensation of the difference of ionic radius between Ca and Ce.

Use of Flue Gas Desulfurization Gypsum as an Activator for a Ground Granulated Blast Furnace Slag (고로슬래그 자극재로써 건식 및 습식 배연탈황석고의 활용가능성 평가)

  • Lee, Hyun-Suk;Kim, Ji-Hyun;Lee, Jae-Yong;Chung, Chul-Woo
    • Journal of the Korea Institute of Building Construction
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    • v.17 no.4
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    • pp.313-320
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    • 2017
  • Flue gas desulfurization gypsum(FDG) is produced when removing sulfur oxides from combustion gas generated by coal power plant. However, the recycling of FDG is still limited to the certain purposes. In order to expand the possible application of FDG, this study aims to utilize FDG as an activator for ground granulated blast furnace slag. FDG produced by dry- and wet-process were used for the experiments. Slag paste specimens were produced by mixing with deionized water and simulated pore solution, and the role of FDG as an activator for blast furnace slag was evaluated using hydration study by XRD analysis and compressive strength development. According to the results, dry-type FDG was found to work as an activator for blast furnace slag without the presence of soluble alkalis. However, wet-type FDG needs assistance by soluble alkalis in order to work as an activator for blast furnace slag. It was also found that the substitution of dry- and wet-type FDG into blast furnace slag can increase the 28 day compressive strength of slag paste. It is expected that efficient and economical recycling of FDG will be possible if quantitative analysis of strength enhancement according to substitution rate of both dry- and wet-type FDG.

Geochemical Modeling on Water-caprock-gas Interactions within a CO2 Injected in the Yeongil Group, Pohang Basin, Korea (포항분지 영일층군 내 이산화탄소 주입에 의한 물-덮개암-가스 반응에 대한 지화학적 모델링)

  • Kim, Seon-ok;Wang, Sookyun;Lee, Minhee
    • Economic and Environmental Geology
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    • v.54 no.1
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    • pp.69-76
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    • 2021
  • This study is to identify the mineralogical properties of caprock samples from drilling cores of the Pohang basin, which is the research area for the demonstration-scale CO2 storage project in Korea. The interaction of water-rock-gas that can occur due to CO2 injection was identified using geochemical modeling. Results of mineralogical studies, together with petrographic data of caprock and data on the physicochemical parameters of pore water were used for geochemical modeling. Modelling was carried out using the The Geochemist's Workbench 14.0.1 geochemical simulator. Two steps of modeling enabled prediction of immediate changes in the caprocks impacted by the first stage of CO2 injection and the assessment of long-term effects of sequestration. Results of minerlaogical analysis showed that the caprock samples are mainly composed of quartz, K-feldspar, plagioclase and a small amount of pyrite, calcite, kaolinite and montmollonite. After the injection of carbon dioxide, the porosity of the caprock increased due to the dissolution of calcite, and dawsonite and chalcedony were precipitated as a result of the dissolution of albite and k-feldspar. In the second step after the injection was completed, the precipitation of dawsonite and chalcedony occurred as a result of dissolution of calcite and albite, and the pH was increased due to this reaction. Results of these studies are expected to be used as data to quantitatively evaluate the efficiency of mineral trapping capture in long-term storage of carbon dioxide.

Experimental Study on the Geochemical and Mineralogical Alterations in a Supercritical CO2-Groundwater-Zeolite Sample Reaction System (초임계 이산화탄소-지하수-제올라이트 시료 반응계에서의 지화학적 및 광물학적 변화에 관한 실험적 연구)

  • Park, Eundoo;Wang, Sookyun;Lee, Minhee
    • Economic and Environmental Geology
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    • v.47 no.4
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    • pp.421-430
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    • 2014
  • In this study, a series of autoclave experiments were conducted in order to investigate the geochemical and mineralogical effects of carbon dioxide on deep subsurface environments. High pressure and temperature conditions of $50^{\circ}C$ and 100 bar, which are representative environments for geological $CO_2$ sequestration, were created in stainless-steel autoclaves for simulating the interactions in the $scCO_2$-groundwater-mineral reaction system. Zeolite, a widespread mineral in Pohang Basin where many researches have been focused as a candidate for geological $CO_2$ sequestration, and groundwater sampled from an 800 m depth aquifer were applied in the experiments. Geochemical and mineralogical alterations after 30 days of $scCO_2$-groundwater-zeolite sample reactions were quantitatively examined by XRD, XRF, and ICP-OES investigations. The results suggested that dissolution of zeolite sample was enhanced under the acidic condition induced by dissolution of $scCO_2$. As the cation concentrations released from zeolite sample increase, $H^+$ in groundwater was consumed and pH increases up to 10.35 after 10 days of reaction. While cation concentrations showed increasing trends in groundwater due to dissolution of the zeolite sample, Si concentrations decreased due to precipitation of amorphous silicate, and Ca concentrations decreased due to cation exchange and re-precipitation of calcite. Through the reaction experiments, it was observed that introduction of $CO_2$ could make alterations in dissolution characteristics of minerals, chemical compositions and properties of groundwater, and mineral compositions of aquifer materials. Results also showed that geochemical reactions such as cation exchange or dissolution/precipitation of minerals could play an important role to affect physical and chemical characteristics of geologic formations and groundwater.

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.

Relationship between Physicochemical Properties, Heavy Metal Contents and Magnetic Susceptibility of Soils (토양의 물리화학적 특성, 중금속 함량, 대자율 간의 상호관계 연구)

  • Chon, Chul-Min;Park, Jeong-Sik;Kim, Jae-Gon;Lee, Youn-Soo
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.4
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    • pp.281-295
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    • 2010
  • This paper deals with magnetic susceptibility, mineralogy, soil properties (pH, EC, CEC, loss on ignition), iron and manganese oxides, the content and partitioning of heavy metals (As, Cd, Cr, Cu, Ni, Pb, Zn), and their mutual relationship in the soil samples of an unpolluted, abandoned mine area, and industrial complex area. The various minerals derived from weathered bedrock were identified by X-ray diffraction in the unpolluted soil samples, except for the magnetic minerals. XRD analysis also revealed the existence of hematite and magnetite related to mine tailings and waste rocks in the abandoned mine area samples. The industrial complex area samples had carbonate minerals, such as calcite and dolomite, that might be due to anthropogenic deposition. The sum of the reducible, oxidizable, and residual fractions was over 80% for the abandoned mine area samples and over 50% for the industrial complex area samples using the sequential extraction method. The industrial complex area samples had a relatively high carbonate fraction that was associated with carbonate minerals. The content of aqua regia-extractable Fe, Mn, As, and Zn had a high positive correlation with the content of the dithionite-citrate-bicarbonate (DCB)-extractable method related to Fe/Mn oxide phases. The 54% and 58% of aqua regia-extractable Fe and As content, respectively, acted together with the concentrations of the DCB-extractable phases. Magnetic susceptibility values of total samples ranged from 0.005 to $2.131{\times}10^{-6}m^3kg^{-1}$. The samples including iron oxide minerals, such as hematite and magnetite, had a high magnetic susceptibility. The magnetic susceptibility showed a significant correlation with the heavy metals, Cd (r=0.544, p<0.05), Cr (r=0.714, p<0.01), Ni (r=0.645, p<0.05), Pb (r=0.703, p<0.01), and Zn (r=0.496, p<0.01), as well as Fe (r=0.608, p<0.01) and Mn (r=0.615, p<0.01). The aqua regia-extractable Fe and Mn content had a significant positive correlation with Cd, Cr, Cu, Ni, and Zn. However, the DCB-extractable Fe and Mn content had a significant positive correlation with As and Ni, indicating that the heavy metals were associated with Fe and Mn oxide minerals.

Primer Evaluation for the Detection of Toxigenic Microcystis by PCR (독소 생성 Microcystis 검출을 위한 PCR primer의 평가)

  • 이현경;김준호;유순애;안태석;김치경;이동훈
    • Korean Journal of Microbiology
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    • v.39 no.3
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    • pp.166-174
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    • 2003
  • Microcystin produced by cyanobacteria in surface waters, such as eutrophic lake and river, is a kind of serious environmental problems due to its toxicity to human and wild animals. Microcystin is synthesized nonribosomally by the large modular multi-functional enzyme complex known as microcystin synthetase encoded by the mcy gene cluster. Amplification of mcy genes by PCR from cultures and environmental samples is a simple and efficient method to detect the toxigenic Microcystis. In order to evaluate primers designed to detect toxic microcystin-producing strains, 17 cyanobacterial strains and 20 environmental samples were examined by PCR with 7 pairs of primers. Some microcystin-producing cyanobacteria were not detected with FAA-RAA, TOX4F-TOX4R and FP-RP primers. The fragment of unexpected size was amplified with NSZW2-NSZW1 primers in Microcystis strains isolated from the lakes in Korea. TOX1P-TOX1F primers failed in amplification of toxin-producing strains. Only MSF-MSR and TOX2P- TOX2F primers amplified the fragments of mcy genes from 11 strains of microcystin-producing Microcystis. The water samples taken from 20 lakes in Korea were analyzed by PCR using each of the primers. In all the water samples, cyanobacteria capable of producing microcystin were detected by the PCR with TOX2P-TOX2F primers. These results indicate that TOX2P-TOX2F primers are better than the other primers for detection of microcystin-producing Microcystis strains in Korea. The nucleotide sequences of mcy gene in Microcystis aeruginosa NIER10010 suggest genetic diversity of Korean isolates.