• Title/Summary/Keyword: R2R XRD

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Synthesis and Crystal Chemistry of New Actinide Pyrochlores (새로운 파이로클로어의 합성 및 결정화학적 특징)

  • ;;;Sergey V. Yudintsev
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.1
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    • pp.78-84
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    • 2002
  • New pyrochlore-type phases($A_2$$B_2$$O_{7}$) were synthesized in the systems: CaO-C$eO_2$-T$iO_2$, CaO-$UO_2$(T$hO_2$)-Z$rO_2$, CaO-$UO_2$(T$hO_2$)-$Gd_2$$O_3$-T$iO_2$-Z$rO_2$, 및 CaO-T$hO_2$-S$nO_2$. The starting materials were pressed with the pressure of 200~400 MPa and sintered at 1500~ 155$0^{\circ}C$ for 4~8 hours in air and at 1300~ 135$0^{\circ}C$ for 5 ~50 hours under oxygen atmosphere. The products were characterized using XRD, SEM/EDS and TEM. In the bulk compositions of CaCe$Ti_2$$O_{7}$, CaTh$Zr_2$$O_{7}$,($Ca_{0.5}$ Gd$Th_{0.5}$)(ZrTi)$O_{7}$) ($Ca_{0.5}$Gd$Th_{0.5}$)(ZrTi)$O_{7}$, ($Ca_{0.5}$G$dU_{0.5}$)(ZrTi)$O_{7}$ and CaTh$Sn_2$$O_{7}$ , pyrochlore was the major phase, together with other oxide phase $of_2$$O_{7}$ fluorite structure. In the samples with target compositions CaU$Zr_2$$O_2$$Ca_{0.5}$ G$dU_{0.5}$)$Zr_2$T$iO_{7}$ pyrochlore was not identified, but a fluorite-structured phase was detected. The formation factor as the stable phase depended on crystal chemical characteristics of the actinide and lanthanide elements of the system concerned.

Dielectric Properties and Microstructure Observation of Complex Perovskite (1-x)$(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$(LNST) system [1] (복합 페로브스카이트 (1-x)$(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$(LNST) system의 유전특성 및 미세구조 관찰 [1])

  • Son, Jin-Ok;Lee, Hwack-Joo;Nahm, Sahn
    • Applied Microscopy
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    • v.34 no.1
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    • pp.61-69
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    • 2004
  • The microwave dielectric properties and microstructures of the Complex Perovskite (1-x)$(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$(LNST) system were investigated using the X-ray diffraction (XRD) and scanning electron microscopy (SEM). LNST had not only the antiphase tilting of oxygen octahedron but also the inphase tilting of oxygen octahedron and the antiparallel shift of cations. Also, when $0.0{\leq}x{\leq}0.4$, LNST had the vacancy ordering of A-sites because of the evaporation of Li ions. From the observation of the microstructure, abnormal grain growth phenomena were observed over the whole range of x. The temperature coefficient of resonant frequency ($T_{cf}$) of the $({Li_{1/2}}^{+1}{Sm_{1/2}}^{+3})TiO_3$(LST) system has a large negative value ($-220ppm/^{\circ}C$) but the $({Na_{1/2}}^{+1}{Sm_{1/2}}^{+3})TiO_3$(NST) system which substituted $Na^{+1}$ has a large positive value ($+173ppm/^{\circ}C$). The dielectric properties of ${\varepsilon}_r=103,\;Q*f_{0}=3,700GHz$ and $T_{cf}=+50ppm/^{\circ}C$ at 4GHz were obtained when x =0.4.

${SO_4}^{2-}$ ion Removal from Solution by Crystal Precipitation on Surface Active Glasses (표면활성유리에의 결정석출을 이용한 용액중 황산염 이온 제거)

  • 남명식;김철영
    • Journal of the Korean Ceramic Society
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    • v.35 no.12
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    • pp.1286-1293
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    • 1998
  • ${SO_4}^{2-}$ ions present in industrial waste water if combined with other metal ions in the water can cause serious scale problem in a transporting pipe. In this study therefore ${SO_4}^{2-}$ ions in an acidic solution have been removed by using surface active glasses. Glasses with various compositions of $SiO_2-Na_2O-B_2O_3-RO$ (R=Mg, Ca, Sr, Ba) system were reacted in a ${SO_4}^{2-}$ ion-containing solution with various pHs ranging from 1 to 4 for various time the reacted glass surfaces were analyzed by XRD and SEM and all ions in the reacted solution were also measured ${SO_4}^{2-}$ ions in the solution were combined with divalent ions leached out of glass and precipitated on the glass surface as sulfate crystals. In this was the surface ion could be removed from the acidic solution. The sulfate ion removal capacity is closely related to the solubility product con-stants of the newly formed sulfate crystals. Almost no sulfate crystal was formed on the MgO-containing glass while sulfate crystals were easily formed on the glass containing either SrO or BaO This indicates that those glasses have strong removal efficiency of ${SO_4}^{2-}$ ions from the solution.

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Attenuation of Chlorinated Pesticides(2,4-D, atrazine) Using Organoclays (유기점토를 이용한 유기염소계 농약(2,4-D, atrazine) 오염 저감)

  • Choi, Ji-Yeon;Shin, Won-Sik
    • Journal of Environmental Science International
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    • v.20 no.2
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    • pp.185-197
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    • 2011
  • Sorption of chlorinated pesticides such as 2,4-dichlorophenoxyacetic acid (2,4-D) and atrazine onto natural clays (montmorillonite and zeolite) modified with cationic surfactant, hexadecyltrimethyl-ammonium (HDTMA) and a natural soil was investigated using batch adsorbers. The clays were transformed from hydrophilic to hydrophobic by the cation exchange between clay surface and HDTMA up to 100% of the cation exchange capacity (CEC). Physicochemical characteristics of the sorbents such as pH, PZC (point of zero charge), organic carbon content ($f_{oc}$), fourier transform infrared spectroscopy (FT-IR), differential thermogravimetric analysis (DTGA) and X-ray diffraction (XRD) were analyzed. Sorption isotherm models such as Freundlich and Langmuir were fitted to the experimental data, resulting Langmuir model ($R^2$ > 0.986) was fitted better than Freundlich model ($R^2$ > 0.973). Sorption capacity ($Q^0$) for 2,4-D and atrazine was in the order of HDTMA-montmorillonite > HDTMA-zeolite > natural soil corresponding to the increase in organic carbon content ($f_{oc}$). The sorption of the pesticides was also affected by pH. The sorption of 2,4-D decreased with the increase in pH, whereas that of atrazine was not changed. This indicated that the sorption capacity ($Q^0$) of 2,4-D and atrazine was not affected by the solution pH because they exist as anionic (deprotonated) forms at pH above pKa. The results indicate that organoclay has a promising potential to reduce chlorinated pesticides in the effluent from golf courses.

Synthesis of Sialon by Carbothermal Reduction of Porous Glass (다공질유리의 탄소 열적환원반응에 의한 Sialon의 합성에 관한 연구)

  • 김병호;이덕열;김왕섭;전형우;이근헌
    • Journal of the Korean Ceramic Society
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    • v.26 no.6
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    • pp.771-782
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    • 1989
  • Synthesis of $\beta$-Sialon powder was attempted with carbothermal reduction of porous glass. The porous glass was prepared by heat and hydrothermal treatments of 9.32 Li2O.46.5B2O3.37.2SiO2.6.98Al2O3 glass. Carbon pyrolyzed from propane gas was deposited on the porous glass, thereafter activated carbon was added as reducing agents. The synthesized $\beta$-Sialon powder was pressureless sintered at 175$0^{\circ}C$ for 1hr in N2 atmosphere. The characterization of the $\beta$-Sialon powder was performed with XRD, BET, SEM and particle size analysis. The sinterability and mechanical properties of the sintered bodies were investigated in terms of bulk density, M.O.R., fracture toughness, morphology of microstructure and etc. The reduction effect of deposited carbon was better than that of activated carbon mechanically added. The formation of SiC was precominant over that of Si2ON2 and $\beta$-Sialon owing to low partial pressure of N2 inside the pore, wehreas on the surface of porous glass the formation of Si2ON2 and $\beta$-Sialon were predominant. Thereafter, SiC reduced unreacted glass to be $\beta$-Sialon. Single phase of $\beta$-Sialon(Z=1.92) was obtained from PGA porous glass having the largest pore radius by the simultaneous reduction and nitridation method at 145$0^{\circ}C$ for 5hrs. The bulk density, M.O.R., and KIC of the sitered body are 3.17g/cc, 434.4MPa and 4.1MPa.m1/2, respectively.

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Physicochemical properties of different phases of titanium dioxide nanoparticles

  • Dong, Vu Phuong;Yoo, Hoon
    • International Journal of Oral Biology
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    • v.46 no.3
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    • pp.105-110
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    • 2021
  • The physicochemical properties of crystalline titanium dioxide nanoparticles (TiO2 NPs) were investigated by comparing amorphous (amTiO2), anatase (aTiO2), metaphase of anatase-rutile (arTiO2), and rutile (rTiO2) NPs, which were prepared at various calcination temperatures (100℃, 400℃, 600℃, and 900℃). X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses confirmed that the phase-transformed TiO2 had the characteristic features of crystallinity and average size. The surface chemical properties of the crystalline phases were different in the spectral analysis. As anatase transformed to the rutile phase, the band of the hydroxyl group at 3,600-3,100 cm-1 decreased gradually, as assessed using Fourier transform infrared spectroscopy (FT-IR). For ultraviolet-visible (UV-Vis) spectra, the maximum absorbance of anatase TiO2 NPs at 309 nm was blue-shifted to 290 nm at the rutile phase with reduced absorbance. Under the electric field of capillary electrophoresis (CE), TiO2 NPs in anatase migrated and detected as a broaden peak, whereas the rutile NPs did not. In addition, anatase showed the highest photocatalytic activity in an UV-irradiated dye degradation assay in the following order: aTiO2 > arTiO2 > rTiO2. Overall, the phases of TiO2 NPs showed characteristic physicochemical properties regarding size, surface chemical properties, UV absorbance, CE migration, and photocatalytic activity.

Study on Physical and Chemical Properties of CaO-Al2O3 System Melting Compound (CaO-Al2O3계 용융화합물의 물리·화학적 특성에 관한 연구)

  • Lee, Keun-Jae;Koo, Ja-Sul;Kim, Jin-Man;Oh, Sang-Yoon
    • Journal of the Korea Concrete Institute
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    • v.25 no.2
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    • pp.209-215
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    • 2013
  • This study is aimed to identify the method to use the CaO-$Al_2O_3$ system of rapidly cooled steel making slag (RCSS) as the environment-friendly inorganic accelerating agent by analyzing its physical and chemical properties. The fraction of rapidly cooled steel making slag is distinguished from its fibrous, and the contents of CaO and $Fe_2O_3$ are inversely proportional across different fractions. In addition, as the content of CaO decreased and the content of $Fe_2O_3$ increased, the loss ignition tended to become negative (-) and the density increased. The pore distribution by mercury intrusion porosimetry is very low as compared to the slowly cooled steel-making slag, which indicates that the internal defect and the microspore rate are remarkably lowered by the rapid cooling. To analyze the major minerals the rapidly cooled steel-making slag, XRD, f-CaO quantification and SEM-EDAX analysis have been performed. The results shows that f-CaO does not exist, and the components are mainly consisted of $C_{12}A_7$ and reactive ${\beta}-C_2S$.

The Study on Dielectric and RTA Property of Oxide Thin-films (산화물 박막 커패시터의 RTA 처리와 유전 특성에 관한 연구)

  • Kim, I.S.;Lee, D.Y.;Cho, Y.R.;Song, J.S.
    • Proceedings of the KIEE Conference
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    • 2001.11a
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    • pp.23-25
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    • 2001
  • In this work, the $Ta_2O_5$ thin films were deposited on Pt/n-Si substrate by reactive magnetron sputtering and the RTA treatment at temperatures range from 650 to $750^{\circ}C$ in $O_2$ and vacuum. X-ray diffraction analysis, FE SEM, dielectric properties and leakage current density have been used to study the structural and electrical properties of the $Ta_2O_5$ thin films. XRD result showed that as- deposited films were amorphous and the annealed films crystallized (<$700^{\circ}C$) into ${\beta}-Ta_2O_5$. The crystallinity increased with temperature in terms of an increase in the intensity of the diffracted peaks(${\beta}-Ta_2O_5$) and annealing in oxygen reduced defect dang1ing Ta-O bonds. As deposited $Ta_2O_5$ films show the leakage current density $10^{-7}$ to $10^{-8}$ (A/$cm^2)$ at low electric fields (<200 kV/cm) However, it was found leakage current density of $Ta_2O_5$ thin films decreased with $O_2$ ambient annealing. The dielectric constant of the as deposited $Ta_2O_5$ thin films was ${\varepsilon}_r$ $9{\sim}11$ but the dielectric constant was increased after RTA treatment in $O_2$ ambient more then in vacuum.

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Optimization of MOF-801 Synthesis Using Sequential Design of Experiments (순차적 실험계획법을 이용한 MOF-801 합성공정 최적화)

  • Lee, Min Hyung;Yoo, Kye Sang
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.621-626
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    • 2021
  • A sequential design of experiments was used to optimize MOF-801 synthesis process. For the initial screening, a general 2k factorial design was selected followed by the central composition design, one of the response surface methods. A 23 factorial design based on the molar ratio of fumaric acid, dimethylformamide (DMF), and formic acid was performed to select the more suitable response variable for the design of experimental method among the crystallinity and BET specific surface area of MOF-801. After performing 8 synthesis experiments designed by MINITAB 19 software, the characteristic analysis was performed using XRD analysis and nitrogen adsorption method. The crystallinity with R2 = 0.999 was found to be more suitable for the experimental method than that of BET specific surface area. Based on analysis of variance (ANOVA), it was confirmed that the molar ratio of fumaric acid and formic acid was a major factor in determining the crystallinity of MOF-801. Through the response optimization and contour plot of two factors, the optimal molar ratio of ZrOCl2·8H2O : fumaric acid : DMF : formic acid was 1 : 1 : 39 : 35. In order to optimize the synthesis process, the central composition design on synthesis time and temperature was performed under the identical molar ratio of precursors. The results derived through the designed 9 synthesis experiments were calculated using the quadratic model equation. Thus, the maximum crystallinity of MOF-801 predicted under the synthesis time and temperature of 7.8 h and 123 ℃, respectively.

Structural and optical properties of sputtered vanadium pentoxide thin films (스퍼터링으로 퇴적시킨 바나듐 산화막의 구조적, 광학적 특성)

  • Choi, Bok-Gil;Shin, Kyu-Ho;Jung, Sang-Jin;Choi, Chang-Kyu;Kim, Sung-Jeen
    • Proceedings of the KIEE Conference
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    • 1998.11c
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    • pp.746-748
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    • 1998
  • Thin films of vanadium pentoxide ($V_{2}O_{5}$) have been deposited by r.f. magnetron sputtering from $V_{2}O_{5}$ target in gas mixture of argon and oxygen. Crystal structure, surface morphology, surface composition and optical properties of films prepared under different substrates are characterized through XRD, SEM, AES, XPS and optical absorption measurements. The films prepared below $100^{\circ}C$ are amorphous, and those prepared above $200^{\circ}C$ are polycrystalline. Thermally Induced oxidation of films into higher oxide has been observed with increasing substrate temperature. Vanadium oxide films show two optical absorption bands indicating the presence of direct and indirect transitions.

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