• Title/Summary/Keyword: High-temperature XRD

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The Structural Stability and Electrochemical Properties of Fe Doped Li[Ni0.575Co0.1Mn0.325]O2 (Fe을 도핑한 Li[Ni0.575Co0.1Mn0.325]O2의 구조적인 안정성 및 전기화학적 특성)

  • Yang, Su-Bin;Yoo, Gi-Won;Jang, Byeong-Chan;Son, Jong-Tae
    • Journal of the Korean Electrochemical Society
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    • v.17 no.3
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    • pp.149-155
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    • 2014
  • In this study, a positive-electrode material in a lithium secondary battery $Li[Ni_{0.575}Co_{0.1}Mn_{0.325}]O_2$ was synthesized as precursor by co-precipitation. Cathode material was synthesized by adding iron. The synthesized cathode material was analyzed by scanning electron microscope and x-ray diffraction. The analysis of x-ray diffraction showed that the a-axis and c-axis is increased by doping iron. And $I_{(003)}/I_{(104)}$ is increased and $I_{(006)}+I_{(102)}/I_{(101)}$ is decreased. Through this result, it was confirmed that the structural stability is improved. And impedance measurements show that the charge transfer resistance ($R_{ct}$) is lowered by doping iron. Consequently, electrochemical properties are improved by doping iron. In particular, the cycle characteristics are improved at a high temperature condition (328 K). Structural stabilities are contributing to the cycle properties.

Mössbauer Studies of Changed Interaction on Cr Ions in Chromite (Chromite 물질의 자기상호작용에 관한 뫼스바우어 분광연구)

  • Choi, Kang-Ryong;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.47-50
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    • 2007
  • [ $ZnCr_2O_4$ ] shows geometrically frustrated magnet. Recently, $CoCr_2O_4$ has been investigated for multiferroic property and dielectric anomalies by spin-current model. Polycrystalline $CoCr_2O_4$ and $CoCrFeO_4$ compounds was prepared by wet-chemical process. Crystallographic and magnetic properties of $CoCr_2O_4$ and $CoCrFeO_4$ were investigate by using the x-ray diffractometer(XRD), vibrating sample magnetometer(VSM), superconducting quantum interference device magnetometer(SQUID), and $M\"{o}ssbauer$ spectroscopy. The crystal structure was found to be single-phase cubic spinel with space group of Fd3m. The lattice constants of $CoCr_2O_4$ and $CoCrFeO_4$ $a_0$ were determined to be 8.340 and 8.377 ${\AA}$, respectively. The ferrimagnetic transition temperature for the both samples were observed at 97 K and 320 K. The $M\"{o}ssbauer$ absorption spectra at 4.2 K show that the well developed two sextets are superposed with small difference of hyperfine field($H_{hf1}=507\;and\;H_{hf2}=492\;kOe$). Isomer shift values($\delta$) of the two sextets are found to be 0.33 and 0.34 mm/s relative to the Fe metal, respectively, which are consistent with the high spin $Fe^{3+}$ charge state.

Effect of composition on the structural and thermal properties of TiZrN thin film (TiZrN 박막의 조성이 구조적 특성 및 열적 특성에 미치는 영향)

  • Choi, Byoung Su;Um, Ji Hun;Seok, Min Jun;Lee, Byeong Woo;Kim, Jin Kon;Cho, Hyun
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.1
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    • pp.37-42
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    • 2021
  • The effect of chemical composition on the structural and thermal properties of TiZrN thin films was studied. As the Zr fraction in the deposited TixZr1-xN (x = 0.87, 0.82, 0.7, 0.6, and 0.28) increased, microstructural changes consisted of reduction in the grain size and a gradual transition from columnar structure to granular structure were observed. In addition, it was also confirmed that a gradual crystal phase transition from TiN to TiZrN has occurred as the Zr fraction increased up to 0.4. After heat treatment at 900℃, Ti0.82Zr0.18N and Ti0.7Zr0.3N layers were converted to a form in which rutile phase TiO2 and TiZrO4 oxides coexist, while Ti0.6Zr0.4N layer was converted to TiZrO4 oxide. Among the five compositions of TiZrN films, the Ti0.6Zr0.4N showed the best high temperature stability and produced a significant enhancement in the thermal oxidation resistance of Inconel 617 through suppressing the surface diffusion of Cr caused by thermal oxidation of the Inconel 617 substrate.

Preparation of NH4+-β"-alumina as a Protonic Solid Electrolyte by Ion Exchange Reaction (이온교환반응에 의한 양성자 고체 전해질 NH4+-β"-alumina의 제조)

  • Lee, Jun-Hee;Han, Choon-Soo;Lee, Sung-Tae;Lee, Ki-Moon;Lee, Dae-Han;Lim, Sung-Ki
    • Applied Chemistry for Engineering
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    • v.22 no.3
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    • pp.255-260
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    • 2011
  • $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina which is expected to an inorganic solid electrolyte of high temperature polymer electrolyte membrane fuel cells (PEMFC) was prepared by ion-exchange reaction of $K^{+}-{\beta}^{{\prime}{\prime}}$-alumina pellet with $NH_4NO_3$ aqueous solution and molten $NH_4NO_3$ salts as an ion-exchange medium in the autoclave and the heating mentle reaction. In the autoclave reaction, the concentrations of $NH_4NO_3$ solution was chosen at 5 and 10 M. Each ion-exchange reaction was carried out at 130, 150, 170, and $200^{\circ}C$ for 2, 4, 6 and 8 h. In the heating mentle reaction, ion-exchange was performed at $200^{\circ}C$ for 2, 4, 6 and 8 h with molten $NH_4NO_3$ salts. In order to determine the effect of reaction times, each ion-exchange reaction was repeated 3 times. The phase stability and the ion-exchange rate of $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina were analyzed by XRD and ICP.

Effects of Sowing Date on Grain Filling and Related Traits in Winter Barley (파종기 차이가 보리의 등숙과 등숙관련 형질에 미치는 영향)

  • 류용환;이창덕;하용웅
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.37 no.1
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    • pp.93-103
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    • 1992
  • Experiments were conducted in the research field of the Wheat and Barley Research Institute with three barley cultivars, Olbori, Kangbori and Suwon 18, which showed different growth characteristics. The highest rates of daily dry matter accumulation in grains were 1.03 1.94 mg / grain / day in early and optimum sowings and 0.88 1.88 mg / grain / day in late sowings, which occurred around 20~30 days after heading in early and optimum sowings and 15~20 days after heading in late sowings. Grains reached their maximum weight by 40 days after heading in early and optimum sowings and 35 days after heading in late sowings. Total sugar content in grains followed a pattern of linear increase immediately after heading, but it started to decrease around 20 days after heading. On the other hand, starch content continued to increase until maturity. The contents of both components were high in the order of 'Olbori' > 'Kangbori' > 'Suwon 18', but they did not respond in a regular pattern to different sowings. 1,000 grain weight showed highly significant positive correlation(r=0.767$^{**}$) with the duration of grain growth, but it had negative correlations with the average (r=-0.548$^{**}$) or the sum (r=-0.595$^{**}$) of post-anthesis daily mean temperature.ature.

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Sorption Efficiency of the Bamboo Charcoal to Remove the Cesium in the Contaminated Water System (오염수계 내 세슘 제거를 위한 대나무 활성탄의 흡착효율 규명)

  • Ahn, Joungpil;Lee, Minhee
    • Economic and Environmental Geology
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    • v.51 no.2
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    • pp.87-97
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    • 2018
  • The cesium (Cs) removal from the contaminated water system has been considered to be difficult because the cesium likes to exist as soluble phases such as ion and complexes than the solid in water system. Many researches have focused on developing the breakthrough adsorbent to increase the cesium removal efficiency in water. In this study, the laboratory scale experiments were performed to investigate the feasibility of the adsorption process using the bamboo charcoal for the Cs contaminated water system. The Cs removal efficiency of the bamboo charcoal were measured and the optimal adsorption conditions were determined by the adsorption batch experiments. Total 5 types of commercialized bamboo charcoals in Korea were used to identify their surface properties from SEM-EDS and XRD analyses and 3 types of bamboo charcoals having large specific surface areas were used for the adsorption batch experiment. The batch experiments to calculate the Cs removal efficiency were performed at conditions of various Cs concentration (0.01 - 10 mg/L), pH (3 - 11), temperature ($5-30^{\circ}C$), and adsorption time (10 - 120 min.). Experimental results were fitted to the Langmuir adsorption isotherm curve and their adsorption constants were determined to understand the adsorption properties of bamboo charcoal for Cs contaminated water system. From results of SEM-EDS analyses, the surfaces of bamboo charcoal particles were composed of typical fiber structures having various pores and dense lamella structures in supporting major adsorption spaces for Cs. From results of adsorption batch experiments, the Cs-133 removal efficiency of C type bamboo charcoal was the highest among those of 3 bamboo charcoal types and it was higher than 75 % (maximum of 82 %) even when the initial Cs concentration in water was lower than 1.0 mg/L, suggesting that the adsorption process using the bamboo charcoal has a great potential to remove Cs from the genuine Cs contaminated water, of which Cs concentration is low (< 1.0 mg/L) in general. The high Cs removal efficiency of bamboo charcoal was maintained in a relatively wide range of temperatures and pHs, supporting that the usage of the bamboo charcoal is feasible for various types of water. Experimental results were similar to the Langmuir adsorption model and the maximum amount of Cs adsorption (qm:mg/g) was 63.4 mg/g, which was higher than those of commercialized adsorbents used in previous studies. The surface coverage (${\theta}$) of bamboo charcoal was also maintained in low when the Cs concentration in water was < 1.0 mg/L, investigating that the Cs contaminated water can be remediated up with a small amount of bamboo charcoal.

Characterization of Mineralogical Changes of Chrysotile and its Thermal Decomposition by Heat Treatment (열처리에 따른 백석면의 광물학적 특성 변화와 열분해 과정 연구)

  • Jeong, Hyeonyi;Moon, Wonjin;Roh, Yul
    • Economic and Environmental Geology
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    • v.49 no.2
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    • pp.77-88
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    • 2016
  • Chrysotile is a 1:1 sheet silicate mineral belonging to serpentine group. It has been highlighted studies because of uses, shapes and structural characteristics of the fibrous chrysotile. However, it was designated as Class 1 carcinogen, so high attentions were being placed on detoxification studies of chrysotile. The objectives of this study were to investigate changes of mineralogical characteristics of chrysotile and to suggest detoxification mechanism of chrysotile by thermal decomposition. Samples for this study were obtained from LAB Chrysotile mine in Canada. The samples were heated in air in the range of 600 to $1,300^{\circ}C$. Changes of mineralogical characteristics such as crystal structure, shape, and chemical composition of the chrysotile fibers were examined by TG-DTA, XRD, FT-IR, TEM-EDS and SEM-EDS analyses. As a result of thermal decomposition, the fibrous chrysotile having hollow tube structure was dehydroxylated at $600-650^{\circ}C$ and transformed to disordered chrysotile by removal of OH at the octahedral sheet (MgOH) (Dehydroxylation 1). Upon increasing temperature, it was transformed to forsterite ($Mg_2SiO_4$) at $820^{\circ}C$ by rearrangement of Mg, Si and O (Dehydroxylation 2). In addition, crystal structure of forsterite had begun to transform at $800^{\circ}C$, and gradually grown 3-dimensionally to enstatite ($MgSiO_3$) by recrystallization after the heating above $1,100^{\circ}C$. And then finally transformed to spherical minerals. This study showed chrysotile structure was collapsed about $600-700^{\circ}C$ by dehydroxylation. And then the fibrous chrysotile was transformed to forsterite and enstatite, as non-hazardous minerals. Therefore, this study indicates heat treatment can be used to detoxification of chrysotile.

Preparation and Characterization of $Cu/Ce_xZr_{1-x}O_2$ Catalysts for Preferential Oxidation of Carbon Monoxide (일산화탄소의 선택적 산화반응을 위한 $Cu/Ce_xZr_{1-x}O_2$ 촉매의 합성과 특성분석)

  • Lee, So-Yeon;Lee, Suk-Hee;Cheon, Jae-Kee;Woo, Hee-Chul
    • Clean Technology
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    • v.13 no.1 s.36
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    • pp.54-63
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    • 2007
  • Even traces of CO in the hydrogen-rich feed gas to proton exchange membrane fuel cells (PEMFC) poison the platinum anode electrode and dramatically decrease the power output. In this work, a variety of catalytic materials consisting of $Cu/Ce_xZr_{1-x}O_2$, (x = 0.0-1.0) were synthesised, characterized and tested for CO oxidation and preferential oxidation of CO (PROX). These catalysts prepared by hydrothermal and deposition-precipitation methods. The catalysts were characterized by XRD, XRF, SEM, BET, $N_2O$ titration and oxygen storage capacity (OSC) measurement. The effects of composition of the support and degree of excess oxygen were investigated fur activity and $CO_2$ selectivity with different temperatures. The composition of the support markedly influenced the PROX activity. Among the various $Cu/Ce_xZr_{1-x}O_2$ catalysts having different composition, $Cu/Ce_{0.9}Zr_{0.1}O_2$ and $Cu/Ce_{0.7}Zr_{0.3}O_2$ showed the highest activities (>99%) and selectivities (ca.50%) in the temperature range of $150{\sim}160^{\circ}C$. It was found that by using of $Ce_xZr_{1-x}O_2$ mixed oxide support which possesses a high oxygen storage capacity, oxidation-reduction activity of Cu-based catalyst was improved, which resulted in the increase of catalytic activity and selectivity of CO oxidation in excess $H_2$ environments.

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Investigations on the Adsorption Characteristics of $SO_2$ Gas on Fixed Bed Manganese Nodule Column (고정(固定) 흡착층(吸着層)에서 망간단괴(團塊)의 $SO_2$ 가스 흡착(吸着) 특성(特性)에 관한 연구(硏究))

  • Baek, Mi-Hwa;Kim, Dong-Su;Jung, Sun-Hee;Park, Kyoung-Ho
    • Resources Recycling
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    • v.15 no.4 s.72
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    • pp.3-12
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    • 2006
  • The feasibility for the employment of manganese nodule as an adsorbent for $SO_{2}$ gas has been investigated. The specific surface area of manganese nodule particle, which used in the experiments, was ca. $221.5m^{2}/g$ and the content of sulfur in manganese nodule was observed to significantly increase after $SO_{2}$ was adsorbed on it. The EPMA for the distilled water-washed and methanol-washed manganese nodule particle after $SO_{2}$ adsorption showed that its sulfur content was slightly decreased to 14.7% and 13.1% respectively, from 15.4% before washing. The XRD analysis of manganese nodule showed that todorokite and birnessite, which are manganese oxides, and quartz and anorthite were the major mineralogical components and weak $MnSO_{4}$ peaks were detected after $SO_{2}$ was adsorbed on manganese nodule. For an comparative investigation, limestone was also tested as an adsorbent for $SO_{2}$, however, no peaks for $CaSO_{4}$ were found by XRD analysis after the adsorption of $SO_{2}$. As the size of adsorbent increased, time for breakthrough was decreased and the adsorbed amount of $SO_{2}$ was also diminished. The $SO_{2}$ adsorption was hindered when its flow rate became high and the adsorption capacity of manganese nodule was observed to be superior to that of limestone. In addition, the mixture of manganese nodule and limestone did not show an increase in the adsorption of $SO_{2}$. Finally, as the temperature was raised, the adsorbed amount of adsorbate on manganese nodule was found to be decreased.

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.