• Title/Summary/Keyword: X-ray Structure Analysis

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Synthesis and Characterization of Magnetic Nanoparticles and Its Application in Lipase Immobilization

  • Xu, Jiakun;Ju, Caixia;Sheng, Jun;Wang, Fang;Zhang, Quan;Sun, Guolong;Sun, Mi
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2408-2412
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    • 2013
  • We demonstrate herein the synthesis and modification of magnetic nanoparticles and its use in the immobilization of the lipase. Magnetic $Fe_3O_4$ nanoparticles (MNPs) were prepared by simple co-precipitation method in aqueous medium and then subsequently modified with tetraethyl orthosilicate (TEOS) and 3-aminopropyl triethylenesilane (APTES). Silanization magnetic nanoparticles (SMNP) and amino magnetic nanomicrosphere (AMNP) were synthesized successfully. The morphology, structure, magnetic property and chemical composition of the synthetic MNP and its derivatives were characterized using transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) analysis, X-ray diffraction, superconducting quantum interference device (SQUID) and thermogravimetric analyses (TGA). All of these three nanoparticles exhibited good crystallization performance, apparent superparamagnetism, and the saturation magnetization of MNP, SMNP, AMNP were 47.9 emu/g, 33.0 emu/g and 19.5 emu/g, respectively. The amino content was 5.66%. The AMNP was used to immobilize lipase, and the maximum adsorption capacity of the protein was 26.3 mg/g. The maximum maintained activity (88 percent) was achieved while the amount of immobilized lipase was 23.7 mg $g^{-1}$. Immobilization of enzyme on the magnetic nanoparticles can facilitate the isolation of reaction products from reaction mixture and thus lowers the cost of enzyme application.

Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.11
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

Manufacturing and Characterization of PVDF/TiO2 Composite Nano Web with Improved β-phase (β-phase가 향상된 PVDF/TiO2 Nano Web 제조 및 특성 분석)

  • Bae, Sung Jun;Kim, Il Jin;Lee, Jae Yeon;Sur, Suk-Hun;Choi, Pil Jun;Sim, Jae Hak;Lee, Seung Geol;Ko, Jae Wang
    • Textile Coloration and Finishing
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    • v.32 no.3
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    • pp.167-175
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    • 2020
  • In this study, the optimum conditions for manufacturing PVDF nano web according to various electrospinning conditions such as solution concentration and applied voltage conditions were confirmed. The optimum spinning conditions were studied by analyzing the changes in the radioactivity of PVDF/TiO2 nano web according to the TiO2 content and the content of β-phase closely related to the piezoelectric properties under established conditions. As a result, it was confirmed that the concentration of the spinning solution was 20 wt%, the applied voltage was 25 kV, and the TiO2 content was 5 phr. PVDF nano web and PVDF/TiO2 nano web were observed morphologies through Scanning Electron Microscope(SEM) analysis. Formation of β-phase by electrospinning was confirmed by Fourier transform infrared spectroscopy(FT-IR) and X-ray Diffractometer(XRD), and the effect of the trapped nano web structure on the piezoelectric properties was investigated.

Crystallographic Analysis of Ar Encapsulate within Cs3-A Zeolite

  • Lim, Woo Taik;Kim, Bok Jo;Park, Jong Sam;Chang, Chang Hwan;Jung, Sung Wook;Heo, Nam Ho
    • Analytical Science and Technology
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    • v.15 no.6
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    • pp.540-549
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    • 2002
  • The arrangement of encapsulated Ar atoms in the molecular-dimensioned cavities of fully dehydrated zeolite A of unit-cell composition $Cs_3Na_8HSi_{12}Al_{12}O_{48}$ ($Cs_3$-A) has been studied crystallographically to probe the confinement effect of guest species in microporous environment. Atoms of Ar were encapsulated in the cavities of $Cs_3$-A by treatment with 410 atm of Ar at $400^{\circ}C$ for two days, followed by cooling at room temperature. The crystal structure of $Cs_3Na_8H$-A(4Ar) ($P_e$ = 410 atm, $a=12.245(2){\AA}$, $R_1=0.0543$, and $R_2=0.0552$) has been determined by single crystal X-ray diffraction technique in the cubic space group $Pm\bar{3}m$ at 21 (1) $^{\circ}C$ and 1 atm. Encapsulated Ar atoms are distributed in three crystallographic distinct positions: 1.5 Ar atoms per unit cell opposite 6-rings, 1.5 opposite four-rings in the large cavity, and finally 1.0 in the sodalite-unit. The possible structures of argon clusters, such as $Ar_2$, $Ar_3$, and $Ar_4$, are proposed.

Characteristics of amorphous indium tin oxide films on PET substrate grown by Roll-to-Roll sputtering system (저온 Roll-to-Roll 스퍼터 시스템을 이용하여 PET 기판위에 성막 시킨 ITO 박막의 전기적, 광학적, 구조적 특성)

  • Cho, Sung-Woo;Bae, Jung-Hyeok;Choi, Kwang-Hyuk;Moon, Jong-Min;Jeong, Jin-A;Jeong, Soon-Wook;Kim, Han-Ki
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.380-381
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    • 2007
  • This paper reports on the deposition conditions and properties of ITO films used as electrode layer in a organic light emitting diodes on a PET substrate. The deposition technique employed was specially designed roll-to-roll sputtering. The oxide was deposited at room temperature in an argon and oxygen plasma on a transparent conducting ITO layer on a PET film. The influence of deposition parameters such as DC power, working pressure and oxygen partial pressure has been investigated, in order to obtain the best compromise between a high deposition rate and adequate electro-optical properties. Electrical and optical properties of ITO films were analyzed by Hall measurement examinations with van der pauw geometry at room temperature and UV/Vis spectrometer analysis, respectively. In addition, the structural properties and surface smoothness were measured by x-ray diffraction and scaning electron microscopy, respectively. From optimized ITO films grown by roll-to-roll sputter system, good electrical$(6.44{\times}10^{-4}\;{\Omega}-cm)$ and optical(above 86 % at 550 nm) properties were obtained. Also, the ITO films exhibited amorphous structure and very flat surface beacause of low deposition temperature.

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Microstructure properties with variation of doped amount $Pr_{2}O_{3}$ of BSCT ceramics ($Pr_{2}O_{3}$ 첨가량에 따른 BSCT 세라믹의 미세구조 특성)

  • Noh, Hyun-Ji;Lee, Sung-Gap;Park, Sang-Man;Yun, Sang-Eun;Kim, Ji-Eun;Lee, Young-Hie
    • Proceedings of the KIEE Conference
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    • 2007.07a
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    • pp.1283-1284
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    • 2007
  • The barium strontium calcium titanate((Ba,Sr,Ca)$TiO_3$) powders prepared by the sol-gel method and $MnCO_3$ as acceptor were mixed oxide method. The microstructure was investigated with variation of $Pr_{2}O_{3}$ amount. The BSCT powder and $Pr_{2}O_{3}$ were mixed with organic vehicle(Ferro. B75001). BSCT thick films were fabricated by the screen-printing method on alumina substrates. The bottom electrode was Pt and upper electrode was Ag, respectively. All BSCT thick films were sintered at $1420^{\circ}C$, for 2h. The result of the differential thermal analysis(DTA), exothermic peak at around $654^{\circ}C$ due to the formation of the polycrystalline perovskite phase. In the X-ray diffraction(XRD) patterns, all BSCT thick films showed the typical perovskite polycrystalline structure and no pyrochlore phase was dbserved. The microstructure investigated by scanning electron microscope(SEM). Pore and grain size of BSCT thick films were decreased with increasing amount of $Pr_{2}O_{3}$ dopant. And the average grain size and thickness of BSCT thick films doped with 0.1 mol% $Pr_{2}O_{3}$ was $3.09{\mu}m$, $60{\mu}m$, respectively. The relative dielectric constant decreased and dielectric loss decreased with increasing amount of $Pr_{2}O_{3}$ dopant, the values of the BSCT thick films no doped with $Pr_{2}O_{3}$ were 7443 and 4 % at 1 kHz, respectively.

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Biotic and Abiotic Reduction of Goethite (α-FeOOH) by Subsurface Microorganisms in the Presence of Electron Donor and Sulfate (전자공여체와 황산염 이용 토착미생물에 의한 침철석(α-FeOOH) 환원 연구)

  • Kwon, Man Jae;Yang, Jung-Seok;Shim, Moo Joon;Lee, Seunghak;Boyanov, Maxim;Kemner, Kenneth;O'Loughlin, Edward
    • Journal of Soil and Groundwater Environment
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    • v.19 no.1
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    • pp.54-62
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    • 2014
  • To better understand dissimilatory iron and sulfate reduction (DIR and DSR) by subsurface microorganisms, we investigated the effects of sulfate and electron donors on the microbial goethite (${\alpha}$-FeOOH) reduction. Batch systems were created 1) with acetate or glucose (donor), 2) with goethite and sulfate (acceptor), and 3) with aquifer sediment (microbial source). With 0.2 mM sulfate, goethite reduction coupled with acetate oxidation was limited. However, with 10 mM sulfate, 8 mM goethite reduction occurred with complete sulfate reduction and x-ray absorption fine-structure analysis indicated the formation of iron sulfide. This suggests that goethite reduction was due to the sulfide species produced by DSR bacteria rather than direct microbial reaction by DIR bacteria. Both acetate and glucose promoted goethite reduction. The rate of goethite reduction was faster with glucose, while the extent of goethite reduction was higher with acetate. Sulfate reduction (10 mM) occurred only with acetate. The results suggest that glucose-fermenting bacteria rapidly stimulated goethite reduction, but acetate-oxidizing DSR bacteria reduced goethite indirectly by producing sulfides. This study suggests that the availability of specific electron donor and sulfate significantly influence microbial community activities as well as goethite transformation, which should be considered for the bioremediation of contaminated environments.

New Evaluation of Initial Growth Mechanisms of Hydroxyapatite on Self-assembled Collagen Nanofibrils by Using ToF-SIMS and AFM Techniques

  • Park, Young-Jae;Choi, Gyu-Jin;Lee, Tae-Geol;Lee, Won-Jong;Moon, Dae-Won
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.397-397
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    • 2010
  • Bone is considered as hierarchically organized biocomposites of organic (collagen) and inorganic (hydroxyapatite) materials. The precise structural dependence between hydroxyapatite (HAp, $Ca_{10}(PO_4)_6(OH)_2)$ crystals and collagen fibril is critical to unique characteristics of bone. To meet those conditions and obtain optimal properties, it is essential to understand and control the initial growth mechanisms of hydroxyapatite at the molecular level, such as other nano-structured materials. In this study, collagen fibrils were prepared by adsorbing native type I collagen molecules onto hydrophobic surface. Hydrophobicity was introduced on the Si wafer surface by using PECVD (plasma enhanced chemical vapor deposition) method and cyclohexane as a precursor. Biomimetic nucleation and growth of HAp on the self-assembled collagen nanofibrils were occurred through incubation of the sample in SBF (simulated body fluid). Chemical and morphological evolution of HAp nanocrystals was investigated by surface-sensitive analytical techniques such as ToF-SIMS (Time-of-Flight Secondary Ion Mass Spectrometry) and AFM (Atomic Force Microscopy) in the early growth stages (< 24 hrs). The very initial stages (< 12 hrs) of mineralization could be clearly demonstrated by ToF-SIMS chemical mapping of surface. In addition to ToF-SIMS and AFM measurement, scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction analysis were conducted to characterize the HAp layer in the late stages. This study is of great importance in the growth of real bone-like materials with a structure analogous to that of natural bones and the development of biomimetic nanomaterials.

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Patterns of Calcification in Thyroid Nodules; Significance and Malignant Potentiality (갑상선결절내 석회화소견과 갑상선암종과의 연관성)

  • Choi Jong-Ouck;Lee Jae-Yong;Chung Keun;Choi Geun
    • Korean Journal of Head & Neck Oncology
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    • v.13 no.1
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    • pp.30-34
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    • 1997
  • Objectives: Calcification of the thyroid nodule has been reported to have a close relationship with differentiated thyroid carcinoma, however there are limited studies on the relationship between the calcified thyroid nodule and thyroid malignancy. The authors studied the clinical significance of calcification within the thyroid nodule. Materials and Methods: There were total of 60 patients who underwent surgery for calcified thyroid nodules which were identified from plain neck X-ray, ultrasound and computed tomography during the period January 1991 to June 1996 at the Department of Otorhinolaryngology-Head and Neck Surgery of Korea University Hospital. Six patients were not included because of recurrence and previous thyroid surgery. Histopathologic and radiologic analysis was done on the remaining 54 patients. Results: Results showed that 25 of 54 cases(46%) to be malignant histopathologically. Of the 25 malignant cases, papillary carcinoma was the most common with 22 cases followed by 2 cases of undifferentiated carcinoma and I case of medullary carcinoma. Statistically high incidence of malignancy was observed when the consistency of calcified thyroid nodule was solid, shape of calcification was irregular and inhomogenous, and adhesion of calcified thyroid nodule to the regional structure was present. Conclusion: The probability that a thyroid nodule is malignant has been reported to be 3­20%. However, about half of the thyroid nodules with calcification found to be malignant on this study, calcification of the thyroid nodule can be used as a guideline for detecting thyroid malignancy.

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Characteristics of NbN Films Deposited on AISI 304 Using Inductively Coupled Plasma Assisted DC Magnetron Sputtering Method

  • Jun, Shinhee;Kim, Junho;Kim, Sunkwang;You, Yong Zoo;Cha, Byungchul
    • Journal of the Korean institute of surface engineering
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    • v.46 no.5
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    • pp.187-191
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    • 2013
  • Niobium nitride (NbN) films were deposited on AISI 304 stainless steels by inductively coupled plasma (ICP) assisted dc magnetron sputtering method at different ICP powers, and the effects of ICP power on the phase formation, mechanical and chemical properties of the films were investigated. X-ray diffraction analysis (XRD) and field emission scanning electron microscopy (FESEM) were used to analyze the crystal structure and micro-knoop hardness was used to measure the hardness of the films. Also, 3-D mechanical profiler and a ball-on-disk wear tester were used to measure the thickness of the films and to estimate wear characteristics, respectively. The thickness of the films decreased but their hardness increased with increasing ICP power, and it was confirmed that only cubic ${\delta}$-NbN(200) remained at high ICP power. At lower ICP powers, a mixture of the hexagonal ${\delta}^{\prime}$-NbN and cubic ${\delta}$-NbN phases was obtained in the films and the hardness decreased. The corrosion potential value increased gradually with increasing ICP power, but the changes of ICP power did not significantly influence the overall corrosion resistance.