• 제목/요약/키워드: X-ray회절법

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Studies on the growth and properties of orthophosphate crystals by the hydrothermal method (수열법에 의한 올소인산염 결정의 육성과 성질에 관한 연구)

  • Pan-Chae Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.2
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    • pp.139-147
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    • 1994
  • Orthophosphate crystals were grown by the hydrothermal method and the properties of grown crystals were investigated by means of X-ray diffraction. Vickers hardness tester, etc. The starting powders of $AIPO_4 and GaPO_4 $were prepared as a single phase by the solid state reaction of stoichiometric mixture of $AI_2O_3 or Ga_2O_3$ and $NH_4H_2PO_4$ and the subsequently by the hydrothermal treatment. The hydrothermal conditions for high growth rates of the orthophosphate crystals are as follows: $AlPO_4$ crystal; temperature ranges, between $170$~$200^{\circ}C$; temperatures difference, $15$~$20^{\circ}C;$, hydrothermal solvent, 4m HCl, $GaPO_4 crystal; temperature ranges, between $210 and 240^{\circ}C;$; temperature difference, $25$~$30^{\circ}C; $, hydrothermal solvent, 4m HCl. Morphologies of grown crystals tended to be bounded by (1010), (1011) and (0111) faces at low temperatures, and grew with well developed (0001) faces by increasing the growth temperature. On the other hand, the properties of orthophosphate crystals $(AlPO_4/GaPO_4)$ were as follows: lattice parameters (nm); a=0.494, c=1.094/a=0.490, c=1.105, density (gcm-3); 2.62/3.56, Vickers hardness (Nm^2); $1.02{\times}10^1^0/7.06{\times}10^9$, refractive indices; $ne=1.529{\pm}0.003, no=1.519{\pm}0.003/ne=1.611{\pm}0.006, no=1.599{\pm}0.006, birefringence; {\pm}0.01/{\pm}0.012$, dielectric constant (Fm-1); 6/7.

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$M\"{o}ssbauer$ Studies by a Heat Treatment in $CoFe_2O_4$ (열처리에 따른 $CoFe_2O_4$$M\"{o}ssbauer$ 분광학적 연구)

  • 이승화;김철성
    • Journal of the Korean Magnetics Society
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    • v.6 no.2
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    • pp.67-72
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    • 1996
  • The crystallographic and magnetic properties of the ferrimagnetic $CoFe_2O_4$ have been studied by X-ray and Mossbauer measurements. The crystal structure is found to be cubic spinel structure with the lattice constant $a_{0}=8.381{\pm}0.005{\AA}\;and\;a_{0}=8.391{\pm}0.005{\AA}$ for slow-cooled and quenched CoFeZ04' respectively. Mossbauer spectra of $CoFe_2O_4$ have been taken at various temperatures ranging from 13 to 780 K. The isorrer shifts indicate that the valence states of the Fe ions for tetrahedral(A) and octahedral(B) sites have ferric character. Debye temperatures for the A and B sites are found to be ${\theta}_A=734{\pm}5K\;and\;{\theta}_B=248{\pm}5K$ for slow-cooled and ${\theta}_A=531{\pm}5K\;and\;{\theta}_B=197{\pm}5K$ for quenched, respectively. Atomic migration from the A to the B sites starts near 400 K and 350 K for slow-cooled and quenched $CoFe_2O_4$, respectively, am increases rapidly with increasing temperature to such a degree that about 69 % for slow-cooled and 91 % for quenched of the ferric ions on the A sites have rmved over to the B sites at 700 K.

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The Growth of $MgO:LiNbO_3$ Single Crystal by Czochralski Method and its Density Measurement (Czochralski법에 의한 $MgO:LiNbO_3$단결정 성장과 밀도 측정)

  • Kim, Il-Won;Park, Bong-Chan;Kim, Gap-Jin
    • Korean Journal of Crystallography
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    • v.4 no.2
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    • pp.74-85
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    • 1993
  • Single crystals of LiNbO3 have found extensive application in electro-optic and nonlinear optic devices. However, laser-induced refartive index inhomogeneities, which have been labeled opical damage impose limits on device optical damage in LiNbO3 is imporved if more than 4.5 rml% MgO is added to the melt The laser damage thrueshold increased as much as 100 times better then that of undoped crystals. The MgO doped cystal has thus been urterlsiv81y studied since then. In the study, Mgo:LiNbOs(MLA) single crystals dopsd with 0, 2.5, 5.0, 7.5, 10.0 mol% MgO have been grown by the czocrualski technique. The metls were prepared in the platinum crluible and 15∼20mm diameter crystals were grown with a length of 20∼30mm in a resitance heater. The growth rate was 2.5mm/hr, the rotation speed 15rpn. Before sawing MLN single crystals were annealed for 24 hours under atmosphere at a temperature of 1080℃. After sawing, we have found an annual ring cross section of MNA crystals only in the direction of perpendicilar to the c-axis. Nonuniform dispusion of MgO was pointed out that the cuties of the state of oxide were strongly affected by oxygen partial pressure in.

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Study on Ionic Conductivity and Crystallinity of PEO/PMMA Polymer Composite Electrolytes containing $TiO_2$ Filler ($TiO_2$ 필러를 포함하는 PEO/PMMA 고분자 복합체 전해질의 이온전도도 및 결정화도)

  • Lee, Lyun-Gyu;Park, Soo-Jin;Kim, Seok
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.758-763
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    • 2011
  • In this work, polymer composite electrolytes were prepared by a blend of poly(methyl methacrylate) (PMMA) and poly(ethylene oxide) (PEO) as a polymer matrix, propylene carbonate as a plasticizer, $LiClO_4$ as a salt, and by containing a different content of $TiO_2$, by using the solution casting method. The crystallinity and ionic conductivity of the polymer electrolytes was evaluated using X-ray diffraction(XRD) and AC impedance method, respectively. The morphology of composite electrolyte film was analyzed by SEM method. From the experimental results, by increasing the $TiO_2$ content, crystallinity of PEO was reduced, and ionic conductivity was increased. In particular, the ionic conductivity was dependent on the content of $TiO_2$ and showed the highest value 15 wt%. However, when $TiO_2$ content exceeds 15 wt%, the ionic conductivity was decreased. According to the surface morphology, the ionic conductivity was decreased because the polymer composite electrolytes showed a heterogenous morphology of fillers due to immiscibility or aggregation of the filler within the polymer matrix.

Suitability evaluation of magnesium substituted biphasic calcium phosphates prepared by coprecipitation method (공침법을 이용한 마그네슘이 첨가된 biphasic calcium phosphate의 적합성 평가)

  • Lee, Hyoung-Sin;Kim, Tae-Wan;Kim, Dong-Hyun;Park, Hong-Chae;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.5
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    • pp.237-242
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    • 2010
  • Magnesium-substituted BCP (biphasic calcium phosphate) powders were prepared by incorporating small amounts of magnesium into the structure of different hydroxyapatite (HAp)/${\beta}$-tricalcium phosphate (${\beta}$-TCP) ratios through coprecipitation method. A series of magnesium substitutions ranging from 0, 0.5, and 1.0 wt%, which are comparable to the measured magnesium contents, were performed. The obtained powders were characterized by the following analytical techniques: X-ray diffraction analysis (XRD), Thermo Gravimetric Analyzer (TGA) and Fourier transform infrared spectroscopy (FT-IR). The results have shown that substitution of magnesium in the calcium-deficient apatites resulted in the formation of biphasic mixtures of different HAP/${\beta}$-TCP ratios after heating above $1000^{\circ}C$. The 1.0 wt% magnesiumsubstituted-BCP were soaked in Hank's solutions after 2 weeks to observe the morphology of the biocement, especially needle-like hydroxyapatite crystals and to estimate the length and diameter of nanoneedle crystals.

Effect of Ratio of Polyoxalate/PLGA Microspheres on the Release Behavior of Zaltoprofen (Polyoxalate 및 PLGA 미립구의 혼합 비율별에 따른 Zaltoprofen의 방출거동)

  • Lee, Jung Keun;Kim, Kyoung Hee;Kim, Young Lae;Park, Guk Bin;Kim, Min Jeong;Kang, Su Ji;Lee, Dongwon;Khang, Gilson
    • Polymer(Korea)
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    • v.37 no.1
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    • pp.28-33
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    • 2013
  • Zaltoprofen, a propionic acid derivative non-steroidal anti-inflammatory drug, was known to have powerful inhibitory effects on acute, subacute and chronic inflammation. For initial release and sustained release, the microspheres were prepared using an emulsion-solvent evaporation method like an O/W emulsion method with varying the ratio of zaltoprofen-loaded polyoxalate (POX)/PLGA micropheres. The morphology of the microspheres was confirmed by scanning electron microscopy. The crystallinity of microspheres was analyzed by X-ray diffraction and differential scanning calorimeter. Fourier transform infrared spectroscopy was used to analyze the chemical structure of microspheres. The increased ratio of POX microspheres affected the initial drug release, and the sustained release of drug was influenced by ratio of PLGA microspheres. In this study, the initial release behavior of zaltoprofen can be controlled by the ratio of POX/PLGA microspheres.

Structural and photoelectrical properties of copper phthalocyanine(CuPc) thin film on Si substrate by thermal evaporation (Si 기판위에 열증착법으로 제조한 copper phthalocyanine(CuPc) 박막의 구조 및 광전특성)

  • Lee, Hea-Yeon;Jeong, Jung-Hyun;Lee, Jong-Kyu
    • Journal of Sensor Science and Technology
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    • v.6 no.5
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    • pp.407-413
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    • 1997
  • The crystallized CuPc(copper phthalocyanine) film on a p-type <100> Si substrate is prepared at the substrate temperature of $300^{\circ}C$ by thermal evaporation. X -ray diffraction analysis showed the CuPc film to have a-axis oriented structure. For the measurement of photovoltaic characteristics of the CuPc/Si film and the Si substrate, a transverse current-voltage (I-V) curve is observed. In the dark, the Au/Si junction is shown to be ohmic contact. However, under illumination, a photovoltaic effect is not observed. The I-V curve in the dark indicates that the CuPc film on Si may form an ohmic contact. Since the CuPc film is a p-type semiconductor, the CuPc/p-Si junction has no barrier at the interface. Under illumination, the CuPc/Si junction shows a large photocurrent comparing with that of the wafer. The result indicates that the CuPc layer plays an important role in the photocarrier generation under red illumination (600 nm). The CuPc/Si film shows the photo voltaic characteristics with a short-circuit photocurrent ($J_{sc}$) of $4.29\;mA/cm^{2}$ and an open-circuit voltage ($V_{oc}$) of 12 mA.

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Preparation and Characterization of Zaltoprofen-Loaded Polyoxalate Microspheres for Control Release (방출제어를 위한 잘토프로펜이 함유된 폴리옥살레이트 미립구의 제조와 특성)

  • Kim, Kyoung Hee;Lee, Cheon Jung;Jo, Sun A;Lee, Jung Hwan;Jang, Ji Eun;Lee, Dongwon;Kwon, Soon Yong;Chung, Jin Wha;Khang, Gilson
    • Polymer(Korea)
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    • v.37 no.6
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    • pp.702-710
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    • 2013
  • Zaltoprofen loaded polyoxalate (POX) microspheres were prepared by an emulsion solvent-evaporation/extraction method like oil-in-water (O/W) for sustained release of zaltoprofen. The influence of several preparation parameters such as fabrication temperature, stirring speed, intensity of the sonication, initial drug ratio, molecular weight ($M_w$) of POX, concentration of POX and concentration of emulsifier has been investigated on the zaltoprofen release profiles. Physicochemical properties and morphology of zaltoprofen loaded POX microspheres were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimeter (DSC) and Fourier transform infrared (FTIR). Through the analyzed results, it was demonstrated that the characteristics of the microspheres greatly affected by the prepared condition. The releases behavior of zaltoprofen was investigated for 10 days in vitro. It was confirmed that the release behavior of zaltoprofen can be controlled by the manufacturing factor of solvent-evaporation/extraction method.

Effect of Cosurfactants on the Release Behavior of Zaltoprofen-loaded PLGA Microspheres in In Vitro : Preparation and Characterization (보조계면활성제 첨가에 따른 잘토프로펜을 함유한 PLGA 미립구의 생체외 방출 거동: 제조 및 특성)

  • Eom, Shin;Yoo, Seok-Cheol;Kim, Yong-Ki;Lee, Young-Hyun;Lee, Eun-Yong;Yu, Hyeon;Lee, Dong-Won;Khang, Gil-Son
    • Polymer(Korea)
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    • v.34 no.4
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    • pp.333-340
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    • 2010
  • Zaltoprofen, a propionic acid derivative non-steroidal anti-inflammatory drug (NSAID), is known to have powerful inhibitory effects on acute, subacute and chronic inflammation. We developed poly(lactide-co-glycolide)(PLGA) microspheres loaded with zaltoprofen for sustained controlled delivery using an oil-water solvent evaporation methods by varying PLGA molecular weight and cosurfactant contents. Physicochemical properties and morphology of zaltoprofen-loaded PLGA microspheres were investigated by scanning electron microscope, X-ray diffraction and differential scanning calorimeter. The size of microspheres increased with the molecular weight of PLGA and the content of cosurfactants. The increase of PLGA molecular weight and cosurfactant content decreased the porosity of microspheres, subsequently resulting in the slow drug release. The results demonstrated that the adjustment of PLGA molecular weight and the cosurfactant content allowed us to control the drug release profiles of drug-loaded microspheres.

Highly-permeable Mixed Matrix Membranes Based on SBS-g-POEM Copolymer, ZIF-8 and Ionic Liquid (SBS-g-POEM 공중합체, ZIF-8, 이온성 액체에 기반한 고투과성 혼합 매질 분리막)

  • Kang, Dong A;Kim, Kihoon;Kim, Jong Hak
    • Membrane Journal
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    • v.29 no.1
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    • pp.44-50
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    • 2019
  • In this paper, we developed mixed matrix membranes (MMMs) consisting of SBS-g-POEM block-graft copolymer, ionic liquid (EMIMTFSI) and ZIF-8 nanoparticles to separate a $CO_2/N_2$ gas pair. The SBS-g-POEM is a rubbery block-graft copolymer synthesized through low-cost free-radical polymerization. The EMIMTFSI was dissolved into the SBS-g-POEM matrix and solution synthesized ZIF-8 nanoparticles were also dispersed into the copolymer matrix. The physico-chemical properties of manufactured membranes were characterized by Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray diffraction (XRD), which showed that the components were compatible with each other. The gas separation performance was confirmed by time-lag measurements showing $CO_2$ permeability of 537.0 barrer and $CO_2/N_2$ selectivity of 15.2. The result represents the EMIMTFSI and ZIF-8 nanoparticles improves the gas permeability more than two-times, without significantly sacrificing the $CO_2/N_2$ selectivity.