• Title/Summary/Keyword: x-Ray diffraction (XRD)

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Effect of Precipitator and Quantity on the Formation of Fe3(PO4)2 (Fe3(PO4)2 생성에 미치는 침전제와 첨가량의 영향)

  • An, Suk-Jin;Lee, Sun-Young;Oh, Kyoung-Hwan;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.587-591
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    • 2011
  • The effect of the precipitator (NaOH, $NH_4OH$) and the amount of the precipitator (150, 200, 250, 300 ml) on the formation of $Fe_3(PO_4)_2$, which is the precursor used for cathode material $LiFePO_4$ in Li-ion rechargeable batteries was investigated by the co-precipitation method. A pure precursor of olivine $LiFePO_4$ was successfully prepared with coprecipitation from an aqueous solution containing trivalent iron ions. The acid solution was prepared by mixing 150 ml $FeSO_4$(1M) and 100 ml $H_3PO_4$(1M). The concentration of the NaOH and $NH_4OH$ solution was 1 M. The reaction temperature (25$^{\circ}C$) and reaction time (30 min) were fixed. Nitrogen gas (500 ml/min) was flowed during the reaction to prevent oxidation of $Fe^{2+}$. Single phase $Fe_3(PO_4)_2$ was formed when 150, 200, 250 and 300 ml NaOH solutions were added and 150, 200 ml $NH_4OH$ solutions were added. However, $Fe_3(PO_4)_2$ and $NH_4FePO_4$ were formed when 250 and 300 ml $NH_4OH$ was added. The morphology of the $Fe_3(PO_4)_2$ changed according to the pH. Plate-like lenticular shaped $Fe_3(PO_4)_2$ formed in the acidic solution below pH 5 and plate-like rhombus shaped $Fe_3(PO_4)_2$ formed around pH 9. For the $NH_4OH$, the pH value after 30 min reaction was higher with the same amount of additions of NaOH and $NH_4OH$. It is believed that the formation mechanism of $Fe_3(PO_4)_2$ is quite different between NaOH and $NH_4OH$. Further investigation on this mechanism is needed. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and the pH value was measured by pH-Meter.

Precipitation Hardening by Holding After Simulated Complete Firing in a Metal-Ceramic Alloy of Pd-Au-Ag-Sn System (금속-세라믹용 Pd-Au-Ag-Sn계 합금의 모의소성 후 계류에 따른 석출경화)

  • Kim, Min-Jung;Shin, Hye-Jung;Kwon, Yong-Hoon;Kim, Hyung-Il;Seol, Hyo-Joung
    • Korean Journal of Dental Materials
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    • v.43 no.4
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    • pp.343-349
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    • 2016
  • This experiment was carried out to examine whether the post-firing heat treatment is effective in increasing the hardness of metal-ceramic alloy of the Pd-Au-Ag-Sn system. Precipitation hardening by holding at $600^{\circ}C$ after simulated complete porcelain firing in a metal-ceramic alloy of the Pd-Au-Ag-Sn system was examined by observing the change in hardness, crystal structure, and microstructure using a hardness test, X-ray diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The hardness of the alloy increased apparently by holding the specimen at $600^{\circ}C$ for 30 min after simulated complete porcelain firing. The formation of fine grain interior precipitates during holding at $600^{\circ}C$ caused the formation of lattice strain in the grain interior, resulting in apparent hardening. The faster cooling rate (stage 0) during simulated complete porcelain firing resulted in more effective precipitation hardening during holding at $600^{\circ}C$. From the above results, an appropriate post-firing heat treatment, such as holding at $600^{\circ}C$ for 30 min after complete porcelain firing may increase the durability of metal-ceramic prostheses composed of Pd-Au-Ag-Sn alloy.

Effect of Hollow Sphere Size on Heat Shield Properties of hollow TiO2/polyacrylate Composites (중공구의 크기에 의한 hollow TiO2/polyacrylate 복합체의 열차단 특성)

  • Kim, Jong Seok
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.690-694
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    • 2021
  • Carbon spheres (CS) were fabricated using glucose as a precursor in the hydrothermal method. Hollow TiO2 (H-TiO2) spheres with 200 nm, 500 nm, and 1,200 nm were synthesized by CS/TiO2 core-shell particles via a sol-gel and calcination method. H-TiO2 spheres with nano and micron sizes were characterized using FE-SEM, HR-TEM, and X-ray diffraction. The CIE color coordinate, solar reflectance, and heat shield temperatures of H-TiO2/polyacrylate (PA) composite film were investigated using a UV-Vis-NIR spectrometer and homemade heat insulation temperature measuring device. H-TiO2/PA composites exhibit excellent thermal insulation since the hollow structure filled with dry air has low thermal conductivity and near infrared light reflecting performance. The thermal insulation increased with increasing the hollow sphere (HS) size on H-TiO2/PA composites. The PA composite film mixed with H-TiO2 filled with 1200 nm HS reduced the heat shield temperature by 26 ℃ compared to that of the transparent glass counterpart.

Behavior of Oxidative Precipitation of High-Arsenic (III) Solution Utilizing Activated Carbon with Air Injection (공기와 활성탄 병용에 의한 용액 중 고농도 3가 비소의 산화-침전 거동 연구)

  • Kim, Rina;Kim, Gahee;Kim, Kwanho;You, Kwang-suk
    • Resources Recycling
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    • v.30 no.4
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    • pp.11-19
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    • 2021
  • Arsenic (As) oxidation followed by precipitation from a high-As(III)-containing leaching solution derived from a sulfidic ore was investigated in this study to remove aqueous As from the solution using activated carbon (AC) with air injection as an oxidant. To obtain the initial leaching solution, a domestic sulfidic ore was leached in a sulfuric acid solution at pH 1 and 50℃ for 95 h, and approximately 7 g/L of Fe and 3 g/L of As were leached out. To determine the effect of the oxidative reaction utilizing AC with air injection, the leaching solution was tested under the following five oxidative conditions at an initial pH of 1 and 90℃ for 72 h: air-only injection; air injection with 1, 5, and 10 w/v% of AC addition; and H2O2 addition. The tests in the presence of both air and AC revealed that the oxidation kinetics and As removal were improved by the reaction between the metallic species and the surface group formed on the AC surface. In addition, the greater the amount of AC added, the better was the reaction efficiency, removing 93-94% of As with more than 5 w/v% of AC addition. Finally, X-ray diffraction analysis confirmed that the precipitate formed from the oxidative reaction was scorodite (FeAsO4·2H2O).

Adsorption of Mn on iron minerals and calcium compounds to reduce Mn(II) toxicity (2가 망간의 독성 저감을 위해 철산화물과 칼슘화합물을 이용한 망간 흡착)

  • Hyo Kyung Jee;Jin Hee Park
    • Journal of Applied Biological Chemistry
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    • v.65 no.4
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    • pp.457-462
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    • 2022
  • Manganese (Mn) exists in various oxidation states and Mn(II) is the most mobile species of Mn, which is toxic to plants and limits their growth. Therefore, the purpose of this study was to reduce Mn toxicity by immobilizing Mn using various adsorbents including iron oxides and calcium compounds. Ferrihydrite, schwertmannite, goethite were synthesized, which was confirmed by X-ray diffraction. Hematite was purchased and used as Mn adsorbent. Calcium compounds such as CaNO3, CaSO4, and CaCO3 were used to increase pH and oxidize Mn. For Mn adsorption, Mn(II) solution was reacted with four iron oxides, CaNO3, CaSO4, and CaCO3 for 24 hours, filtered, and the remaining Mn concentrations in the solution were analyzed by inductively coupled plasma optical emission spectroscopy. The adsorption rate and adsorption isotherm were calculated. Among iron oxides, the adsorption rate was highest for hematite followed by ferrihyrite, but goethite and schwertmannite did not adsorb Mn. In the case of calcium compounds, the adsorption rate was high in the order of CaCO3>CaNO3>CaSO4. In conclusion, treatment of CaCO3 was the most effective in reducing Mn toxicity by increasing pH.

Geotechnical Engineering Characteristics of Ulleung Basin Sediment, East Sea (동해, 울릉 분지 심해토의 지반공학특성)

  • Lee, Chang-Ho;Yun, Tae-Sup;J.C., Santamarina;Bahk, Jang-Jun;Lee, Jong-Sub
    • Journal of the Korean Geotechnical Society
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    • v.25 no.6
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    • pp.17-29
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    • 2009
  • There has been an increase in the investigation of deep sea sediments with a consequent increase in the amount of energy required to undertake these investigations. The geotechnical characteristics of Ulleung Basin sediment are explored by using depressurized specimens following methane production tests carried out on pressured core samples obtained at 2,100 m water depth and 110 m below sea floor. Geotechnical index tests, X-ray diffraction, and scanning electron microscope are conducted to identify the geotechnical index parameters, clay mineralogy, chemical composition, and microstructure of the sediments. Compressibility, and elastic and electromagnetic wave parameters are investigated for two samples by using a multi sensing instrumented oedometer cell. The strength chatracteristics are obtained by the direct shear tests. The dominant clay minerals are mostly kaolinite, illite, chlorite, and calcite. The SEM shows a well-developed flocculated structure of the microfossil. Void ratio, electrical resistivity, real permittivity, conductivity, and shear wave velocity show bi-linear behavior with the effective vertical stress: as the vertical effective stress increases. The friction angle obtained by the direct shear test is about $21^{\circ}$, which is similar to the value observed in the Ulleung Basin sediments. This study shows that the understanding of the behavior acting on the diatomaceous marine sediment is important because it often maintains the useful energy resources such as gas hydrate and so will be the new engineering field in the next generation.

Consolidation and magnetic properties of ferromagnetic Fe-MgO powders prepared by ball milling process (볼밀링법으로 제조된 강자성 Fe-MgO 분말의 벌크화 및 자기적 특성)

  • Chung-Hyo Lee
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.4
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    • pp.125-130
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    • 2024
  • Preparation of ferromagnetic powders for the mixture of hematite and pure Mg powders by ball milling has been investigated. Also, consolidation of the ball-milled powders was performed in a spark plasma sintering machine at 800-1,000℃. It is found that a ferromagnetic Fe-MgO composite powders are obtained by ball milling of hematite and pure Mg powders before 1 hour. The magnetization and coercivity of ball-milled samples change at the results of the solid state reaction of hematite by pure Mg during ball milling. The saturation magnetization of ball-milled samples increases with increasing ball milling time and reaches to a maximum value of 93.4 emu/g after 5 hours of ball milling. Shrinkage change after sintering of ball-milled sample for 5 hours was significant above 300℃ and gradually increased with increasing temperature up to 800℃. X-ray diffraction result shows that the average grain size of Fe in Fe-MgO bulk sample sintered at 900℃ is 50 nm. It can be also seen that the coercivity of bulk sample sintered at 900℃ is still high value of 90 Oe, indicating that the grain growth of magnetic Fe phase during sintering process tend to be suppressed.

Mineral Composition and Grain Size Distribution of Fault Rock from Yangbuk-myeon, Gyeongju City, Korea (경주시 양북면 단층암의 광물 조성과 입도 분포 특징)

  • Song, Su Jeong;Choo, Chang Oh;Chang, Chun-Joong;Chang, Tae Woo;Jang, Yun Deuk
    • Economic and Environmental Geology
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    • v.45 no.5
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    • pp.487-502
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    • 2012
  • This paper is focused on mineral compositions, microstructures and distributional characters of remained grains in the fault rocks collected from a fault developed in Yongdang-ri, Yangbuk-myeon, Gyeongju City, Korea, using X-ray diffraction (XRD), optical microscope, laser grain size analysis and fractal dimension analysis methods. The exposed fault core zone is about 1.5 meter thick. On the average, the breccia zone is 1.2 meter and the gouge zone is 20cm thick, respectively. XRD results show that the breccia zone consists predominantly of rock-forming minerals including quartz and feldspar, but the gouge zone consists of abundant clay minerals such as chlorite, illite and kaolinite. Mineral vein, pyrite and altered minerals commonly observed in the fault rock support evidence of fault activity associated with hydrothermal alteration. Fractal dimensions based on box counting, image analysis and laser particle analysis suggest that mineral grains in the fault rock underwent fracturing process as well as abrasion that gave rise to diminution of grains during the fault activity. Fractal dimensions(D-values) calculated by three methods gradually increase from the breccia zone to the gouge zone which has commonly high D-values. There are no noticeable changes in D-values in the gouge zone with trend being constant. It means that the bulk-crushing process of mineral grains in the breccia zone was predominant, whereas abrasion of mineral grains in the gouge zone took place by continuous fault activity. It means that the bulk-crushing process of mineral grains in the breccia zone was predominant, whereas abrasion of mineral grains in the gouge zone took place by continuous fault activity. Mineral compositions in the fault zone and peculiar trends in grain distribution indicate that multiple fault activity had a considerable influence on the evolution of fault zones, together with hydrothermal alteration. Meanwhile, fractal dimension values(D) in the fault rock should be used with caution because there is possibility that different values are unexpectedly obtained depending on the measurement methods available even in the same sample.

Corrosion Characteristics by CCPP Control in Simulated Distribution System (CCPP 조절에 따른 모의 상수관로의 부식특성에 관한 연구)

  • Kim, Do-Hwan;Lee, Jae-In;Lee, Ji-Hyung;Han, Dong-Yueb;Kim, Dong-Youn;Hong, Soon-Heon
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.12
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    • pp.1249-1256
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    • 2005
  • This study was performed to investigate the efficiency of the corrosion prevention in the simulated distribution system using CCPP(Calcium Carbonate Precipitation Potential) as the anti-corrosive index by adjusting pH, total dissolved solids, alkalinity and calcium hardness in the water treatment pilot process. The materials of the simulated distribution system(SDS) were equiped with same materials of real field water distribution system. CCPP concentrations controlled by $Ca(OH)_2$, $CO_2$ gas and $Na_2CO_3$ in the simulated distribution system and uncontrolled by the chemicals in the general water distribution system were average 0.61 mg/L and -7.77 mg/L. The concentrations of heavy metals like Fe, Zn, Cu ions in effluent water of the simulated distribution system controlled with water quality were decreased rather than the general water distribution system uncontrolled with water quality. In simulated distribution system(SDS), corrosion prevention film formed by CCPP control was observed that scale was come into forming six months later and it was formed into density as time goes on. We were analyzed XRD(X-ray diffraction) for investigating component of crystal compounds and structure for galvanized steel pipe(15 mm). Finding on analysis, scale was compounded to $Zn_4CO_3(OH)_6{\cdot}H_2O$ (Zinc Carbonate Hydroxide Hydrate) after ten months late, and it was compounded on $CaCO_3$(Calcium Carbonate) and $ZnCO_3$(Smithsonite) after nineteen months later.

Identification of Active Agents for Reductive Dechlorination in Cement/Fe(II) Systems (시멘트와 Fe(II)을 이용한 환원성 탈염소화반응의 유효반응성분 규명)

  • Kim, Hong-Seok;Lee, Yu-Jung;Kim, Ha-Yan;Hwang, In-Seong
    • Journal of Soil and Groundwater Environment
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    • v.11 no.6
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    • pp.35-42
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    • 2006
  • Experimental study was conducted to identify the active agent for reductive dechlorination of TCE in cement/Fe(II) systems. Several potential materials-hematite (${\alpha}-Fe_2O_3$), lepidocrocite (${\gamma}$-FeOOH), akaganeite (${\beta}$-FeOOH), ettringite ($Ca_6Al_2(SO_4)_3(OH)_{12}$)-that are cement components or parts of cement hydrates were tested if they could act as reducing agents by conducting TCE degradation experiments. From the initial degradation experiments, hematite was selected as a potential active agent. The pseudo-first-order degradation rate constant ($k\;=\;0.637\;day^{-1}$) for the system containing 200 mM Fe(II), hematite and CaO was close to that ($k\;=\;0.645\;day^{-1}$) obtained from the system containing cement and 200 mM Fe(II). CaO, which was originally added to simulate pH of the cement/Fe(II) system, was found to play an important role in degradation reactions. The reactivity of the hematite/CaO/Fe(II) system initially increased with increase of CaO dosage. However, the tendency declined in the higher CaO dosage region, implying a saturation type of behavior. The SEM analysis revealed that the hexagonal plane-shaped crystals were formed during the reaction with increasing degradation efficiency, which was brought about by increasing the CaO dosage. It was suspected that the crystals could be portlandite or green rust ($SO_4$) or Friedel's salt. The XRD analysis of the same sample identified the peaks of hematite, magnetite/maghemite, green rust ($SO_4$). Either instrumental analysis predicted the presence of the green rust ($SO_4$). Therefore, the green rust ($SO_4$) would potentially be a reactive agent for reductive dechlorination in cement/Fe(II) systems.