• Title/Summary/Keyword: XRD analysis

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A STUDY ON OXIDATION TREATMENT OF URANIUM METAL CHIP UNDER CONTROLLING ATMOSPHERE FOR SAFE STORAGE

  • Kim, Chang-Kyu;Ji, Chul-Goo;Bae, Sang-Oh;Woo, Yoon-Myeoung;Kim, Jong-Goo;Ha, Yeong-Keong
    • Nuclear Engineering and Technology
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    • v.43 no.4
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    • pp.391-398
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    • 2011
  • The U metal chips generated in developing nuclear fuel and a gamma radioisotope shield have been stored under immersion of water in KAERI. When the water of the storing vessels vaporizes or drains due to unexpected leaking, the U metal chips are able to open to air. A new oxidation treatment process was raised for a long time safe storage with concepts of drying under vacuum, evaporating the containing water and organic material with elevating temperature, and oxidizing the uranium metal chips at an appropriate high temperature under conditions of controlling the feeding rate of oxygen gas. In order to optimize the oxidation process the uranium metal chips were completely dried at higher temperature than $300^{\circ}C$ and tested for oxidation at various temperatures, which are $300^{\circ}C$, $400^{\circ}C$, and $500^{\circ}C$. When the oxidation temperature was $400^{\circ}C$, the oxidized sample for 7 hours showed a temperature rise of $60^{\circ}C$ in the self-ignition test. But the oxidized sample for 14 hours revealed a slight temperature rise of $7^{\circ}C$ representing a stable behavior in the self-ignition test. When the temperature was $500^{\circ}C$, the shorter oxidation for 7 hours appeared to be enough because the self-ignition test represented no temperature rise. By using several chemical analyses such as carbon content determination, X-ray deflection (XRD), Infrared spectra (IR) and Thermal gravimetric analysis (TGA) on the oxidation treated samples, the results of self-ignition test of new oxidation treatment process for U metal chip were interpreted and supported.

Evaluation of Fire-induced Damage for Shield Tunnel Linings Subjected to High Temperatures (고온에 노출된 쉴드터널 라이닝의 손상평가)

  • Lee, Chang Soo;Kim, Yong Hyok;Kim, Young Ook
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.16 no.4
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    • pp.1-8
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    • 2012
  • The aim of this study is to evaluate fire-induced damage for shield tunnel linings. Full-scale fire test was conducted to evaluate fire-induced damage. Residual compressive strength was measured on the core samples of shield tunnel lining subjected to high temperatures. Heating temperature was predicted by XRD and TG analysis. As a result, Strength degradation of concrete with temperatures can be evaluated by residual compressive strength of core samples. In addition, residual compressive strength can be estimated by previous studies if heating temperature is exactly predicted. It is possible that heating temperature is predicted by XRD and TG analysis at $450^{\circ}C$. For more accurate prediction of heating temperature it should be performed both instrumental analysis and analytical methods with temperatures ranging from $400{\sim}600^{\circ}C$.

Influence of Reaction Conditions on the Grafting Pattern of 3-Glycidoxypropyl trimethoxysilane on Montmorillonite

  • He, Wentao;Yao, Yong;He, Min;Kai, Zhang;Long, Lijuan;Zhang, Minmin;Qin, Shuhao;Yu, Jie
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.112-116
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    • 2013
  • Surface modification of montmorillonite (MMT) with 3-glycidoxypropyl trimethoxysilane (3GTO) in mild methanol/water mixture has been investigated in detail. The influence of reaction conditions (including silane concentration in feed, reaction time and reaction temperature) on the grafting amount and yield of silane, and further on the grafting pattern of silanes was studied by thermogravimetric analysis, elemental analysis, X-ray diffraction (XRD) and BET. Higher silane concentration, longer reaction time and higher reaction temperature are all benefit to higher grafting amount. When the grafting reaction was performed with 3 mmol/g silane concentration, at $90^{\circ}C$ for 24 h, the grafted amount and yield of silane reached 1.4443 mmol/g and 30%, respectively. Based on the XRD and BET data analysis, a speculation that the grafting pattern of silanes was concentration dependence was proposed.

Isothermal Decomposition of Ammonium Molybdate to Molybdenum Trioxide in a Fluidized Bed Reactor

  • Oh, Chang-Sup;Park, Yong-Ok;Hasolli, Naim;Kim, Hang Goo;Won, Yong Sun;Shin, Su-Been;Kim, Yong-Ha
    • Korean Journal of Materials Research
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    • v.25 no.10
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    • pp.547-551
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    • 2015
  • The present study prepared molybdenum trioxide ($MoO_3$), the most important intermediate of molybdenum metal, by using a fluidized bed reactor for the thermal decomposition of ammonium molybdate (AM) in the presence of an air flow. During the process of fluidizing the sample inside the reactor, the reaction time and temperature were optimized with a close analysis of the X-ray diffraction (XRD) data and with thermogravimetric analysis (TGA). In particular, the temperature level, at which the AM decomposition is completed, is very important as a primary operating parameter. The analysis of the XRD and TGA data showed that the AM decomposition is almost completed at ${\sim}350^{\circ}C$ with a reaction time of 30 min. A shorter reaction time of 10 min. required a higher reaction temperature of ${\sim}500^{\circ}C$ with the same air flow rate to complete the AM decomposition. A sharp rise in the decomposition efficiency at a temperature ranging between 320 and $350^{\circ}C$ indicated a threshold for the AM decomposition. The operating conditions determined in this study can be used for future scale-ups of the process.

Optimization of MOF-235 Synthesis by Analysis of Statistical Design of Experiment (통계학적 실험계획법 해석을 통한 MOF-235 합성 최적화)

  • Chung, Mingee;Yoo, Kye Sang
    • Applied Chemistry for Engineering
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    • v.30 no.5
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    • pp.615-619
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    • 2019
  • Statistical design of experiments was performed to optimize MOF-235 synthesis process. Concentrations of terephthalic acid (TPA), iron (III) chloride hexahydrate, N,N-dimethylformamide (DMF) and ethanol were important factors to develop the crystal structure of MOF-235. MOF-235 was synthesized with various concentrations of the listed chemicals above and the crystallinity was measured by XRD. The effect of the composition on the synthesis of MOF-235 was evaluated using a statistical analysis. For the variance analysis using F-test, the concentration of ethanol showed the greatest effect on the crystallinity and TPA the least influential. A regression model for predicting the crystallinity of MOF-235 was derived and the prediction results for two synthetic variables were presented using contour plots. Finally, the crystallinity was predicted by a mixture method with $FeCl_3$, ethanol and DMF.

Evaluation of Some Stone Dust and Sludge Generated in the Aggregate Production Process and Research Trends for Its Use (골재 생산과정에서 발생하는 일부 석분의 평가와 그 활용 연구 동향)

  • Lee, Jin-Young;Cheong, Young-Wook;Ji, Sang-Woo;Lee, Dong-Gil
    • Economic and Environmental Geology
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    • v.54 no.5
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    • pp.605-613
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    • 2021
  • When crushing rocks to produce aggregates, solid stone dust or sludge is generated as a by-product. These by-products are classified as waste and are not utilized, and most of them are disposed of landfills. This by-product differs in mineral composition, chemical composition, and physical properties depending on the rock type and aggregate production process. Therefore, if a technology that can make good use of the inherent physical or chemical properties of by-products is developed, economic and environmental benefits can be achieved instead of disposal. In this study, stone dust and sludge were collected from domestic aggregate producers and physical and chemical properties were investigated by performing XRD mineral analysis, particle size analysis, and chemical analysis. In addition, the research trend was identified through a domestic and international research case studies on the use of stone powder and sludge.

Analysis of post-annealing effect and electrical properties of Li3PO4/SiC (Li3PO4/SiC의 후열처리에 의한 영향 및 전기적 특성 분석)

  • Lee, Hyung-Jin;Kim, Minkyung;Oh, Jong-Min;Shin, Weon-Ho;Park, Chulhwan;Koo, Sang-Mo
    • Journal of IKEEE
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    • v.26 no.2
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    • pp.232-239
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    • 2022
  • We analyzed the effect of post-annealing on lithium phosphate (Li3PO4) solid-state thin-film. Li3PO4 thin films were deposited by radio frequency (RF) sputtering, with subsequent annealing of the films at 200-400 ℃. SEM imaging of the sample surfaces showed no significant difference in morphology between the annealed and non-annealed samples. XRD analysis indicated that the samples consist of an amorphous-like structure. Post-annealing changes in binding energy were confirmed by XPS analysis, while the leakage current density at -6 V was measured to be about 7.15 times lower in a device that had been annealed at 400 ℃ vs a non-annealed device. It was confirmed that the leakage current decreased with increasing post-annealing temperature.

Hydration Properties of High-strength Cementitious Composites Incorporating Waste Glass Beads (폐유리발포비드를 혼입한 고강도 시멘트 복합체의 수화 특성)

  • Pyeon, Su-Jeong;Kim, Gyu-Yong;Lee, Sang-Soo;Nam, Jeong-Soo
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.10 no.1
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    • pp.74-79
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    • 2022
  • In this study, the effect of a sudden decrease in internal humidity and a decrease in hydration level due to the tight internal structure of high-strength concrete and cement composites was investigated. To verify the change in the internal Si hydration, waste glass foam beads were used as a lightweight aggregate, and the internal unreacted hydrate reduction and hydrate formation tendency were identified over the mid- to long-term. Waste glass foam beads were mixed with 5, 10, and 20 %, and were used by pre-wetting. As the mixing rate of the waste glass foamed beads increased, the strength showed a tendency to decrease. In addition, when the mixing amount of pre-wetted waste glass foam beads increases inside through XRD analysis, TGA analysis, and Si NMR analysis, it is judged that the hydration degree of internal Si is different because moisture is supplied to the paste.

Synthesis and Comparative Analysis of Crystallite Size and Lattice Strain of Pb2Ba1.7Sr0.3Ca2Cu3O10+δ Superconductor

  • Hasan, Maher Abd Ali;Jasim, Kareem Ali;Miran, Hussein Ali Jan
    • Korean Journal of Materials Research
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    • v.32 no.2
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    • pp.66-71
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    • 2022
  • In this article, Pb2Ba1.7Sr0.3Ca2Cu3O10+δ superconductor material was synthesized using conventional solid-state reaction method. X-ray diffraction (XRD) analysis demonstrated one dominant phase 2223 and some impurities in the product powder. The strongest peaks in the XRD pattern were successfully indexed assuming a pseudo-tetragonal cell with lattice constants of a = 3.732, b = 3.733 and c = 14.75 Å for a Pb-Based compound. The crystallite size and lattice strain between the layers of the studied compound were estimated using several methods, namely the Scherrer, Williamson-Hall (W.H), size-strain plot (SSP) and Halder Wagner (H.W) approach. The values of crystallite size, calculated by Scherrer, W.H, SSP and H.W methods, were 89.4540774, 86.658638, 87.7555823 and 85.470086 Å, respectively. Moreover, the lattice strain values obtained by W.H, SSP and H.W methods were 0.0063240, 0.006325 and 0.006, respectively. It was noted that all crystallite size results are consistent; however, the best method is the size-strain plot because it gave a value of R2 approaching one. Furthermore, degree of crystallites was calculated and found to be 59.003321%. Resistivity analysis suggests zero-resistance, which is typical of superconducting materials at critical temperature. Four-probe technique was utilized to measure the critical temperature at onset Tc(onset), zero resistivity Tc(off set), and transition (width ΔT), corresponding to temperatures of 128 K, 116 K, and 12 K, respectively.

Petrographic Study of Mn-bearing Gondite (Birimian) of Téra Area in the Leo-Man Shield (West African Craton) in Niger.

  • Hamidou GARBA SALEY;Moussa KONATE;Olugbenga Akindeji OKUNLOLA
    • Economic and Environmental Geology
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    • v.57 no.1
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    • pp.25-39
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    • 2024
  • The Téra manganese deposit represents the most significant manganese mineralization discovered in Niger up today. The main host rocks of this ore are gondites, which are a garnet and quartz rich metamorphic rocks. The supergene weathering developed an alteration profile on these gondites. This study aims to identify the mineralogical composition of gondites and associated rocks, in order to highlight the origine of rocks and the manganese enrichment. The methodological approach adopted involved a field study followed by polarizing microscopic analysis using transmitted and reflected lights. Additionally, quantitative X-ray diffraction (XRD) analysis was performed to assess the manganese ore minerals present in the gondite and associated rocks, including mica schists, amphibolites, and quartzites. The petrographic study revealed a paragenesis characterized by the presence of kyanite, staurolites, garnets and plagioclases that are generally poikiloblasts with quartz and opaque minerals inclusions, emphasizing the internal schistosity which is planar, helicitic or microfolded. These features indicate a prograde metamorphism until high-pressure amphibolite facies conditions. These conditions are followed by greenschist facies conditions marked by calcite, epidote, muscovite, chlorite and muscovite assemblage which emphasizes the vertical tectonics. Depending on the alteration process, the manganese ore exhibit a granular texture at the bottom of the gondite hills, transitioning to a colloform texture towards the top, passing through the epigenization and replacement texture. The XRD analysis further revealed that the studied rocks originated from a volcano-sedimentary complex, characterized by alternating marly, arenaceous and pelitic sequences associated with submarine exhalations.