• Title/Summary/Keyword: XRD Analysis

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Characteristics of Cement Matrix/Mortar with CaO-based Activated-sludge (CaO원 활성슬러지를 혼입한 시멘트 경화체 및 모르타르의 특성)

  • Lee, Yong-Soo;Ryu, Seong-Lyong;Shin, Kwang-Ho;Chu, Yong-Sik;Kim, Young-Yup
    • Journal of the Korea Concrete Institute
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    • v.29 no.4
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    • pp.399-406
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    • 2017
  • CaO-based by-product, which consist of CaO, $SO_3$, $Al_2O_3$ and so on, has being used to raw materials of CaO compound. When It was applied to recycling water of remicon, concrete performance can be enhanced because hydration reaction of powder material is accelerated. In this study, activated-sludge, which was putted desulfurization gypsum of CaO-based in recycling water, was manufactured to verify effect of them, and then they was investigated by characteristics of cement matrix and mortar. As a results, they indicated reduction of setting time and high soundness in cement matrix, and acceleration of hydration reaction can be verified by XRD analysis. Also, it can be maintained good workability if water content by usage of desulfurization gypsum, which used for production of activated-sludge, was adjusted. In addition, it can be verified strength development by activated-sludge although cement content by usage of desulfurization gypsum was reduced.

Enhanced critical current density of in situ processed MgB2 bulk superconductors with MgB4 additions

  • Kim, S.H.;Kang, W.N.;Jun, B.H.;Lee, Y.J.;Kim, C.J.
    • Progress in Superconductivity and Cryogenics
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    • v.19 no.1
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    • pp.36-41
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    • 2017
  • The effects of $MgB_4$ addition on the superconducting properties and the microstructure of in situ processed $MgB_2$ bulk superconductors were studied. $MgB_4$ powder of 1-20 wt.% was mixed with (Mg + 2B) powder and then pressed into pellets. The pellets of (Mg + 2B + $xMgB_4$) were heat-treated at $650^{\circ}C$ for 1 h in flowing argon. The powder X-ray diffraction (XRD) analysis for the heat-treated samples showed that the major formed phase in all samples was $MgB_2$ and the minor phases were $MgB_4$ and MgO. The full width at half maximum (FWHM) values showed that the grain size of $MgB_2$ decreased as the amount of $MgB_4$ addition increased. $MgB_4$ particles included in a $MgB_2$ matrix is considered to suppress the grain growth of $MgB_2$. The onset temperatures ($T_{c,onset}$) of $MgB_2$ with $MgB_4$ addition (0-10 wt.%) was between 37-38 K. The 20 wt.% $MgB_4$ addition slightly reduced the $T_{c,onset}$ of $MgB_2$ to 36.5 K. This result indicates that $MgB_4$ addition did not influence the superconducting transition temperature ($T_c$) of $MgB_2$ significantly. On the other hand, the small additions of 1-5 wt.% $MgB_4$ increased the critical current density ($J_c$) of $MgB_2$. The $J_c$ enhancement by $MgB_4$ addition is attributed not only to the grain size refinement but also to the possible flux pinning of $MgB_4$ particles dispersed in a $MgB_2$ matrix.

Reaction Characterization of Y2Ba1CU1O5 Oxides by Solid State Reaction Method and Pyrophoric Synthesis Method (고상반응법과 발화합성법에 의한 Y2Ba1CU1O5 산화물의 반응특성)

  • Park, Jeong-Shik
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

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SURFACE CHARACTERISTICS AND BIOLOGICAL RESPONSES OF HYDROXYAPATITE COATING ON TITANIUM BY HYDROTHERMAL METHOD: AN IN VITRO STUDY

  • Kim, Dong-Seok;Kim, Chang-Whe;Jang, Kyung-Soo;Lim, Young-Jun
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.3
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    • pp.363-378
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    • 2005
  • Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.

Effects of Boride on Microstructure and Properties of the Electroconductive Ceramic Composites of Liquid-Phase-Sintered Silicon Carbide System (액상소결(液狀燒結)한 SiC계(系)의 전도성(電導性) 복합체(複合體)의 미세구조(微細構造)와 특성(特性)에 미치는 Boride의 영향(影響))

  • Shin, Yong-Deok;Ju, Jin-Young;Ko, Tae-Hun
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.56 no.9
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    • pp.1602-1608
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    • 2007
  • The composites were fabricated, respectively, using 61[vol.%] SiC-39[vol.%] $TiB_2$ and using 61[vol.%] SiC-39[vol.%] $ZrB_2$ powders with the liquid forming additives of 12[wt%] $Al_2O_3+Y_2O_3$ by hot pressing annealing at $1650[^{\circ}C]$ for 4 hours. Reactions between SiC and transition metal $TiB_2$, $ZrB_2$ were not observed in this microstructure. The result of phase analysis of composites by XRD revealed SiC(6H, 3C), $TiB_2$, $ZrB_2$ and $YAG(Al_5Y_3O_{12})$ crystal phase on the Liquid-Phase-Sintered(LPS) $SiC-TiB_2$, and $SiC-ZrB_2$ composite. $\beta\rightarrow\alpha-SiC$ phase transformation was occurred on the $SiC-TiB_2$ and $SiC-ZrB_2$ composite. The relative density, the flexural strength and Young's modulus showed the highest value of 98.57[%], 249.42[MPa] and 91.64[GPa] in $SiC-ZrB_2$ composite at room temperature respectively. The electrical resistivity showed the lowest value of $7.96{\times}10^{-4}[\Omega{\cdot}cm]$ for $SiC-ZrB_2$ composite at $25[^{\circ}C]$. The electrical resistivity of the $SiC-TiB_2$ and $SiC-ZrB_2$ composite was all positive temperature coefficient resistance (PTCR) in the temperature ranges from $25[^{\circ}C]$ to $700[^{\circ}C]$. The resistance temperature coefficient of composite showed the lowest value of $1.319\times10^{-3}/[^{\circ}C]$ for $SiC-ZrB_2$ composite in the temperature ranges from $100[^{\circ}C]$ to $300[^{\circ}C]$ Compositional design and optimization of processing parameters are key factors for controlling and improving the properties of SiC-based electroconductive ceramic composites.

Solidification of Molten Salt Waste by Gel-Route Pre-treatment (겔화 전처리법을 이용한 폐용융염의 고형화)

  • Park Hwan Seo;Kim In Tae;Kim Hwan Young;Ryu Seung Kon;Kim Joon Hyung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.3 no.1
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    • pp.57-65
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    • 2005
  • This study suggested a new method for the solidification of molten salt waste generated from the electro-metallurgical process in the spent fuel treatment. Using binary material system, sodium silicate and phosphoric acid, metal chlorides were converted into metal phosphate in the micro-reaction module formed by SiO$_{2} particles. The volatile element in the reaction module would little vaporized below 1100$^{circ}$C After the gel product was mixed with borosilicate glass powder and thermally treated at 1000$^{circ}$C, li exists as Li$_{3}$PO$_4$ separated from glass phase and, Cs and Sr would be incorporated into an amorphous phase from XRD analysis. In case of the addition of ZrCl$_{4}$ to the binary system, the gel products were transformed into NZP structure considered as an prospective ceramic waste form after heat-treatment above 700 $^{circ}$C. From these results, the gel-route pretreatment can be considered as an effective approach to the solidincation of molten salt waste by the confirmed process or waste form and this also would be an alternative method on the ANL method using zeolites in USA by the confirmation of its chemical durability as an future work.

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Effects of Aging on Properties of MgO-Partially Stabilized Zirconia (마그네시아 부분안정화 지르코니아 소결체의 특성에 미치는 열처리 효과)

  • 정형진;오영제;이홍림
    • Journal of the Korean Ceramic Society
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    • v.24 no.3
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    • pp.243-250
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    • 1987
  • The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.

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Change of Electrochemical Characteristics Due to the Fe Doping in Lithium Manganese Oxide Electrode

  • Ju Jeh Beck;Kang Tae Young;Cho Sung Jin;Sohn Tae Won
    • Journal of the Korean Electrochemical Society
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    • v.7 no.3
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    • pp.131-137
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    • 2004
  • Sol-gel method which provides better electrochemical and physiochemical properties compared to the solid-state method was used to synthesize the material of $LiFe_yMn_{2-y}O_4$. Fe was substituted to increase the structural stability so that the effects of the substitution amount and sintering temperature were analyzed. XRD was used for the structural analysis of produced material, which in turn, showed the same cubic spinel structure as $LiMn_2O_4$ despite the substitution of $Fe^{3+}$. During the synthesis of $LiFe_yMn_{2-y}O_4$, as the sintering temperature and the doping amount of Fe(y=0.05, 0.1, 0.2)were increased, grain growth proceeded which in turn, showed a high crystalline and a large grain size, certain morphology with narrow specific surface area and large pore volume distribution was observed. In order to examine the ability for the practical use of the battery, charge-discharge tests were undertaken. When the substitution amount of $Fe^{3+}\;into\;LiMn_2O_4$ increased, the initial discharge capacity showed a tendency to decrease within the region of $3.0\~4.2V$ but when charge-discharge processes were repeated, other capacity maintenance properties turned out to be outstanding. In addition, when the sintering temperature was $800\~850^{\circ}C$, the initial capacity was small but showed very stable cycle performance. According to EVS(electrochemical voltage spectroscopy) test, $LiFe_yMn_{2-y}O_4(y=0,\;0.05,\;0.1,\;0.2)$ showed two plateau region and the typical peaks of manganese spinel structure when the substitution amount of $Fe^{3+}$ increased, the peak value at about 4.15V during the charge-discharge process showed a tendency to decrease. From the previous results, the local distortion due to the biphase within the region near 4.15V during the lithium extraction gave a phase transition to a more suitable single phase. When the transition was derived, the discharge capacity decreased. However the cycle performance showed an outstanding result.

Effect of Support Geometry on Catalytic Activity of Pt/CeO2 Nanorods in Water Gas Shift Reaction (Water Gas Shift 반응에서 Pt/CeO2 촉매의 지지체구조에 따른 촉매활성 연구)

  • Im, Hyo Been;Kwon, Soon Jin;Byun, Chang Ki;Ahn, Hee Sung;Koo, Kee Young;Yoon, Wang Lai;Yi, Kwang Bok
    • Journal of Hydrogen and New Energy
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    • v.25 no.6
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    • pp.577-585
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    • 2014
  • Nanorod and particle shape $CeO_2$ were synthesized via hydrothermal process and precipitation method, respectively, and used as supports of Pt catalyst for water gas shift (WGS) reaction. Three different durations (12, 48, and 96h) for hydrothermal process were applied for the preparation of nanorod type $CeO_2$. 1.0 wt% of Pt was loaded on the prepared supports with incipient wetness method prior to the catalytic activity tests that were carried out at a GHSV of $95,541h^{-1}$, and a temperature range of 200 to $360^{\circ}C$. Varying duration of hydrothermal process led to the difference in physical characteristics of $CeO_2$ nanorods, such as aspect ratio, BET surface area, pore diameter, and pore volume. Consequently, the catalytic activities of Pt/$CeO_2$ nanorods were affected by the physical characteristics of the supports and appeared to be in the order of Pt/$CeO_2$(12) > Pt/$CeO_2$(48) > Pt/$CeO_2$(96). The comparison of the catalytic activities and results of the analysis (XPS, XRD, SEM, BET and TPR) for the supports revealed that the activity of the catalysts depends on chemical states of the Pt and the support materials in the temperature range that is lower than $280^{\circ}C$. However, the activity is rather dependent on the physical characteristic of the supports because the increased gas velocity limits the mass transfer of reactants in micropores of the supports.

Growth of Li2B4O7 Single Crystal and Its Thermoluminescent Properties (Li2B4O7 단결정 성장과 열형광 특성)

  • Park, Kang-Soo;Ahn, Jung-Keun;Kim, Dong-Jin;Hwang, Yoon-Hwae;Kim, Hyung-Kook;Park, Myeong-Hwan;Kang, Hee-Dong;Kim, Do-Sung
    • Journal of Sensor Science and Technology
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    • v.12 no.1
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    • pp.16-23
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    • 2003
  • Thermoluminescent properties of $Li_2B_4O_7$ single crystal grown by Czochralski method have been investigated. The high quality $Li_2B_4O_7$ single crystal without core was obtained at rotation speed of 10 rpm for seed crystal and pulling speed below $0.18\;mm{\cdot}h^{-1}$. The structure of $Li_2B_4O_7$ single crystal was classified as tetragonal by XRD analysis. The TL glow curve was composed with three overlapped peaks which can be easily deconvoluted and the TL response of $Li_2B_4O_7$ single crystal TLD to X-ray radiation is linear within the range of $50\;mGy{\sim}1.5\;Gy$. Activation energies of three TL glow peaks analyzed by the various heating rates method and PL spectrum were 0.93, 1.78 and 2.25 eV, respectively.