• Title/Summary/Keyword: High-temperature XRD

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Characterization of NiO-TiO2 Modified with WO3 and Catalytic Activity for Acid Catalysis

  • Pae, Young-Il;Bae, Mu-Hee;Park, Won-Cheon;Sohn, Jong-Rack
    • Bulletin of the Korean Chemical Society
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    • v.25 no.12
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    • pp.1881-1888
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    • 2004
  • A series of $NiO-TiO_2$/$WO_3$ catalysts was prepared by drying powdered $Ni(OH)_2-Ti(OH)_4$ with ammonium metatungstate aqueous solution, followed by calcining in air at high temperature. Characterization of prepared catalysts was performed by using FTIR, Raman, XPS, XRD, and DSC and by measuring surface area. Upon the addition of tungsten oxide to titania up to 25 wt%, the specific surface area and acidity of catalysts increased in proportion to the tungsten oxide content due to the interaction between tungsten oxide and titania. Since the -$TiO_2$/stabilizes the tungsten oxide species, for the samples equal to or less than 25 wt%, tungsten oxide was well dispersed on the surface of titania, but for the samples containing above 25 wt%, the triclinic phase of $WO_3$ was observed at calcination temperature above 400 $^{\circ}C$. The catalytic activities of 10-NiO-$TiO_2$/$WO_3$ for 2-propanol dehydration and cumene dealkylation were correlated with the acidity of catalysts measured by ammonia chemisorption method. NiO may attract reactants and enhance the local concentration of reactants near the acid sites, consequently showing the increased catalytic activities.

XRD study of the layered structure compounds [Zn${(H_2O)}_6$] (${(C_{n}H_{2n+1}SO_3)}_2$ (층상구조인 [Zn${(H_2O)}_6$ (${(C_{n}H_{2n+1}SO_3)}_2$ 화합물에 대한 X-선 회절 연구)

  • 박용준;박양순;이종규;박성훈;전태현;허영덕
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.10 no.4
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    • pp.318-323
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    • 2000
  • The intercalated compounds of alkylsulfonates into hydrated zinc were synthesized. From the high temperature powder X-ray diffraction (HTXRD), FT-IR, and molecular size, the temperature dependence of orientation for the intercalated alkylsulfonates were determined. In the temperatures range 1, alkylsulfonates were intercalated into hexa aqua zinc layer with the bilayer structure of $32.9^{\circ}$angle for ${Zn(H_2O_4]^{2+}[C_nH_{2n+1}SO_3]_2\;^-$. In the temperatures range 2, alkylsulfonates were intercalated into tetra aqua zinc layer with the bilayer structure of $55.2^{\circ}$angle for ${Zn(C_nH_{2n+1}SO_3)_2$. In the temperatures range 3, alkylsulfonates were directly bonded to zinc ion with the bilayer structure of $76.5^{\circ}$angle for ${Zn(C_nH_{2n+1}SO_3)_2$.

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Preparation and Characterization of Solid Dispersions of Itraconazole by using Aerosol Solvent Extraction System for Improvement in Drug Solubility and Bioavailability

  • Lee, Si-Beum;Nam, Kyung-Wan;Kim, Min-Soo;Jun, Seoung-Wook;Park, Jeong-Sook;Woo, Jong-Soo;Hwang, Sung-Joo
    • Archives of Pharmacal Research
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    • v.28 no.7
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    • pp.866-874
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    • 2005
  • The objective of this study was to elucidate the feasibility to improve the solubility and bioavailability of poorly water-soluble itraconazole via solid dispersions by using supercritical fluid (SCF). Solid dispersions of itraconazole with hydrophilic polymer, HPMC 2910, were prepared by the aerosol solvent extraction system (ASES) under different process conditions of temperature/pressure. The particle size of solid dispersions ranged from 100 to 500 nm. The equilibrium solubility increased with decrease (15 to 10 MPa) in pressure and increase (40 to $60^{\circ}C$) in temperature. The solid dispersions prepared at $60^{\circ}C$/15 MPa showed a slight increase in equilibrium solubility (approximately 27-fold increase) when compared to pure itraconazole, while those prepared at $60^{\circ}C$/10MPa showed approximately 610-fold increase and no endothermic peaks corresponding to pure itraconazole were observed, indicating that itraconazole might be molecularly dispersed in HPMC 2910 in the amorphous form. The amorphous state of itraconazole was confirmed by DSC/XRD data. The pharmacokinetic parameters of the ASES-processed solid dispersions, such as $T_{max},\;C_{max},\;and\;AUC_{0-24h}$ were almost similar to $Sporanox_{\circledR}$ capsule which shows high bioavailability. Hence, it was concluded that the ASES process could be a promising technique to reduce particle size and/or prepare amorphous solid dispersion of drugs in order to improve the solubility and bioavailability of poorly water-soluble drugs.

Structural and Optical Properties of ZnO Thin Films Grown on SiO2/Si(100) Substrates by RF Magnetron Sputtering (RF 마그네트론 스퍼터링 방법으로 SiO2/Si(100) 기판위에 성장시킨 ZnO 박막의 구조 및 광특성)

  • Han Seok Kyu;Hong Soon-Ku;Kim Hyo-Jin;Lee Jae-Wook;Lee Jeong-Yong
    • Korean Journal of Materials Research
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    • v.16 no.6
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    • pp.360-366
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    • 2006
  • A series of ZnO thin films were grown by radio-frequency (RF) magnetron sputtering with various RF powers on $SiO_2/Si$(100) substrates at $500^{\circ}C$. Thicknesses of the investigated ZnO films were fixed to about 250nm by changing the growth time based on the changes of growth rates with RF powers. All the ZnO thin films were grown with <0001> preferred orientation. Average grain sizes of about 250nm-thick ZnO films evaluated by FE-SEM, AFM, and TEM were increased by decreasing the RF power. Structural properties addressed by FWHM values of XRD (0002) omega rocking curves and their intensities were better for the smaller grain sized ZnO films grown with high RF powers, which implies small values of tilt for smaller grain sized ZnO films. However, optical properties addressed by intensities of band edge emissions from room temperature and low temperature photoluminescence were better for the larger grain sized ZnO films with low RF power, which implies grain boundaries acted as nonradiation recombination centers.

Thermal Treatment Effect on Thermoelectric Characteristics of Perovskite La0.5Ca0.5MnO3 (페로브스카이트 La0.5Ca0.5MnO3 재료의 열전 특성에 미치는 열처리 효과)

  • Yang, Su-Chul
    • Journal of the Korean Electrochemical Society
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    • v.20 no.3
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    • pp.55-59
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    • 2017
  • In this study, thermoelectric characteristics of perovskite $La_{0.5}Ca_{0.5}MnO_3$ (LCMO) nanomaterials were investigated by theoretical simulation and experimental analysis. Thermoelectric power factors calculated by DFT simulation were gradually enhanced as increase in annealing temperature. Maximum power factor was obtained with high magnitude of $S^2{\sigma}=566{\mu}W/m{\cdot}K^2$ at 1100 K through a dominant improvement of Seebeck coefficient compared with electrical conductivity. Experimentally, the LCMO nanomaterials were hydrothermally synthesized and then treated by post thermal annealing with temperature variation. X-ray diffraction and SEM analysis illustrated that LCMO exhibited orthorhombic perovskite structures with small grain size of 16~19 nm over 873 K. The results directly confirmed that improvement of crystallinity and decrease of mean grain size given by post thermal annealing lead to enhancements of electrical conductivity and Seebeck coefficient, respectively.

Composition Control of a Light Absorbing Layer of CuInSe2 Thin Film Solar Cells Prepared by Electrodeposition (전착법을 이용한 CuInSe2 박막태양전지 광활성층의 조성 조절)

  • Park, Young-Il;Kim, Donghwan;Seo, Kyungwon;Jeong, Jeung-Hyun;Kim, Honggon
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.26 no.3
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    • pp.232-239
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    • 2013
  • Thin light-active layers of the $CuInSe_2$ solar cell were prepared on Mo-coated sodalime glass substrates by one-step electrodeposition and post-annealing. The structure, morphology, and composition of $CuInSe_2$ film could be controlled by deposition parameters, such as the composition of metallic precursors, the concentration of complexing agents, and the temperature of post-annealing with elemental selenium. A dense and uniform Cu-poor $CuInSe_2$ film was successfully obtained in a range of parametric variation of electrodeposition with a constant voltage of -0.5 V vs. a Ag/AgCl reference electrode. The post-annealing of the film at high temperature above $500^{\circ}C$ induced crystallization of $CuInSe_2$ with well-developed grains. The KCN-treatment of the annealed $CuInSe_2$ films further induced Cu-poor $CuInSe_2$ films without secondary phases, such as $Cu_2Se$. The structure, morphology, and composition of $CuInSe_2$ films were compared with respect to the conditions of electrodeposition and post-annealing using SEM, XRD, Raman, AES and EDS analysis. And the conditions for preparing device-quality $CuInSe_2$ films by electrodeposition were proposed.

Effect of Seed-layer thickness on the Crystallization and Electric Properties of SBN Thin Films. (SBN 박막의 결정화 및 전기적 특성에 관한 씨앗층 두께의 영향)

  • Jang, Jae-Hoon;Lee, Dong-Gun;Lee, Hee-Young;Cho, Sang-Hee
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2003.11a
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    • pp.271-274
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    • 2003
  • [ $Sr_xBa_{1-x}Nb_2O_6$ ] (SBN, $0.25{\leq}x{\leq}0.75$) ceramic is a ferroelectric material with tetragonal tungsten bronze (TTB) type structure, which has a high pyroelectric coefficient and a nonlinear electro-optic coefficient value. In spite of its advantages, SBN has not been investigated well compared to other ferroelectric materials with perovskite structure. In this study, SBN thin film was manufactured by ion beam sputtering technique using the prepared SBN target in $Ar/O_2$ atmosphere. SBN30 thin films of different thickness were pre-deposited as a seed layer on $Pt(100)/TiO_2/SiO_2/Si$ substrate followed by SBN60 deposition up to $4500\;{\AA}$ in thickness. As-deposited SBN60/SBN30 layer was heat-treated at different temperatures of 650, 700, 750, and $800\;^{\circ}C$ in air, respectively, The crystallinity and orientation behavior as well as electric properties of SBN60/SBN30 multi-layer were examined. The deposited layer was uniform and the orientation was shown primarily along (001) plane from XRD pattern. There was difference in the crystal structure with heat-treatment temperature, and the electric properties depended on the heating temperature and the seed-layer thickness. In electric properties of Pt/SBN60/SBN30/Pt thin film capacitor prepared, the remnant polarization (2Pr) value was $15\;{\mu}C/cm^2$, the coercive field (Ec) 65 kV/cm, and the dielectric constant 1492, respectively.

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Heavy metal adsorption of a novel membrane material derived from senescent leaves: Kinetics, equilibrium and thermodynamic studies

  • Zhang, Yu;Tang, Qiang;Chen, Su;Gu, Fan;Li, Zhenze
    • Membrane and Water Treatment
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    • v.9 no.2
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    • pp.95-104
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    • 2018
  • Copper pollution around the world has caused serious public health problems recently. The heavy metal adsorption on traditional membranes from wastewater is limited by material properties. Different adsorptive materials are embedded in the membrane matrix and act as the adsorbent for the heavy metal. The carbonized leaf powder has been proven as an effective adsorbent material in removing aqueous Cu(II) because of its relative high specific surface area and inherent beneficial groups such as amine, carboxyl and phosphate after carbonization process. Factors affecting the adsorption of Cu(II) include: adsorbent dosage, initial Cu(II) concentration, solution pH, temperature and duration. The kinetics data fit well with the pseudo-first order kinetics and the pseudo-second order kinetics model. The thermodynamic behavior reveals the endothermic and spontaneous nature of the adsorption. The adsorption isotherm curve fits Sips model well, and the adsorption capacity was determined at 61.77 mg/g. Based on D-R model, the adsorption was predominated by the form of physical adsorption under lower temperatures, while the increased temperature motivated the form of chemical adsorption such as ion-exchange reaction. According to the analysis towards the mechanism, the chemical adsorption process occurs mainly among amine, carbonate, phosphate and copper ions or other surface adsorption. This hypothesis is confirmed by FT-IR test and XRD spectra as well as the predicted parameters calculated based on D-R model.

Electrical Conductivity of the Solid Solutions X $ZrO_2+ (1-X) Yb_2O_3; 0.01{\leq}X{\leq}0.09$

  • Choi Byoung Ki;Jang Joon Ho;Kim, Seong Han;Kim, Hong Seok;Park, Jong Sik;Kim Yoo Young;Kim, Don;Lee Sung Han;Yo Chul Hyun;Kim Keu Hong
    • Bulletin of the Korean Chemical Society
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    • v.13 no.3
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    • pp.248-252
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    • 1992
  • $ZrO_2-dopedYb_2O_3solid$ solutions containing 1, 3, 5, 7 and 9 mol% $ZrO_2were$ synthesized from spectroscopically pure $Yb_2O_3$ and $ZrO_2$ powders and found to be rare earth C-type structure by XRD technique. Electrical conductivities were measured as a function of temperatures from 700 to $1050^{\circ}C$ and oxygen partial pressures from 1${\times}$$10^-5$ to 2${\times}$ $10^-1$atm. The electrical conductivities depend simply on temperature and the activation energies are determined to be 1.56-1.68 $_eV$. The oxygen partial pressure dependence of the electrical conductivity shows that the conductivity increases with increasing oxygen partial pressure, indicating p-type semiconductor. The $PO_2$ dependence of the system is nearly power of 1/4. It is suggested from the linearity of the temperature dependence of electrical conductivity and only one value of 1/n that the solid solutions of the system have single conduction mechanism. From these results, it is concluded that the main defects of the system are negatively doubly charged oxygen interstitial in low. $ZrO_2doping$ level and negatively triply charged cation vacancy in high doping level and the electrical conduction is due to the electronic hole formed by the defect structure.

Effects of the Content of MgO Additive and Sintering Temperature on the Densification of Alumina Insulator (인슐레이터용 알루미나의 치밀화에 미치는 MgO의 함량과 소결 온도의 영향)

  • Ri Joo Kim;Han Gyeol Jeong;Ye Ji Son;Sang Ki Ko;Hyun Seon Hong
    • Journal of Powder Materials
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    • v.30 no.3
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    • pp.249-254
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    • 2023
  • The influence of MgO addition on the densification and microstructure of alumina (Al2O3) was studied. Compacted alumina specimens were manufactured using ball-milling and one-directional pressing followed by sintering at temperatures below 1700℃. Relative density, shrinkage, hardness, and microstructure were investigated using analytical tools such as FE-SEM, EDS, and XRD. When the MgO was added up to 5.0 wt% and sintered at 1500℃ and 1600℃, the relative density exhibited an average value of 97% or more at both temperatures. The maximum density of 99.2% was with the addition of 0.5 wt% MgO at 1500℃. Meanwhile, the specimens showed significantly lower density values when sintered at 1400℃ than at 1500℃ and 1600℃ owing to the relatively low sintering temperature. The hardness and shrinkage data also showed a similar trend in the change in density, implying that the addition of approximately 0.5 wt% MgO can promote the densification of Al2O3. Studying the microstructure confirmed the uniformity of the sintered alumina. These results can be used as basic compositional data for the development of MgO-containing alumina as high-dielectric insulators.