• Title/Summary/Keyword: crystal structure analysis

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Characteristics of $Ta_{2}O_{5}$ Films by RF Reactive Sputtering (RF 반응성 스펏터링으로 제조한 $Ta_{2}O_{5}$ 막의 특성)

  • Park, Wug-Dong;Keum, Dong-Yeal;Kim, Ki-Wan;Choi, Kyu-Man
    • Journal of Sensor Science and Technology
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    • v.1 no.2
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    • pp.173-181
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    • 1992
  • Tantalum pentoxide($Ta_{2}O_{5}$) thin films on p-type (100) silicon wafer were fabricated by RF reactive sputtering. Physical properties and structure of the specimens were examined by XRD and AES. From the C-V analysis, the dielectric constant of $Ta_{2}O_{5}$ films was in the range of 10-12 in the reactive gas atmosphere in which 10% of oxygen gas is mixed. The ratio of Ta : 0 was 1 : 2 and 1 : 2.49 by AES and RBS examination, respectively. The heat-treatment at $700^{\circ}C$ in $O_{2}$ ambient led to induce crystallization. When the heat-treatment temperature was $1000^{\circ}C$, the dielectric constant was 20.5 in $O_{2}$ ambient and 23 in $N_{2}$ ambient, respectively. The crystal structure of $Ta_{2}O_{5}$ film was pseudo hexagonal of ${\delta}-Ta_{2}O_{5}$. The flat band voltage shift(${\Delta}V_{FB}$) of the specimens and the leakage current density were decreased for higher oxygen mixing ratio. The maximum breakdown field was 2.4MV/cm at the oxygen mixing ratio of 10%. The $Ta_{2}O_{5}$ films will be applicable to hydrogen ion sensitive film and gate oxide material for memory device.

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Chimie Douce Synthesis of Chalcogen-Doped Manganese Oxides (칼코겐이 도핑된 망간 산화물의 저온합성 연구)

  • Hwang, Seong-Ju;Im, Seung-Tae;Park, Dae-Hun;Yun, Yeong-Su
    • Journal of the Korean Chemical Society
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    • v.50 no.4
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    • pp.315-320
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    • 2006
  • manganese oxides have been prepared by Chimie Douce redox reaction between permanganate and chalcogen element fine powder under acidic condition (pH = 1). According to powder X-ray diffraction analyses, the S- and Se-doped manganese oxides are crystallized with layered birnessite and tunnel-type -MnO2 structures, respectively. On the contrary, Te-doped compound was found to be X-ray amorphous. According to EDS analyses, these compounds contain chalcogen dopants with the ratio of chalcogen/manganese = 4-7%. We have investigated the chemical bonding character of these materials with X-ray absorption spectroscopic (XAS) analysis. Mn K-edge XAS results clearly demonstrated that the manganese ions are stabilized in octahedral symmetry with the mixed oxidation states of +3/+4. On the other hand, according to Se K- and Te L1-edge XAS results, selenium and tellurium elements have the high oxidation states of +6, which is surely due to the oxidation of neutral chalcogen element by the strong oxidant permanganate ion. Taking into account their crystal structures and Mn oxidation states, the obtained manganese oxides are expected to be applicable as electrode materials for lithium secondary batteries.

3D Printing-Based Ultrafast Mixing and Injecting Systems for Time-Resolved Serial Femtosecond Crystallography (시간 분해 직렬 펨토초 결정학을 위한 3차원 프린팅 기반의 초고속 믹싱 및 인젝팅 시스템)

  • Ji, Inseo;Kang, Jeon-Woong;Kim, Taeyung;Kang, Min Seo;Kwon, Sun Beom;Hong, Jiwoo
    • Korean Chemical Engineering Research
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    • v.60 no.2
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    • pp.300-307
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    • 2022
  • Time-resolved serial femtosecond crystallography (TR-SFX) is a powerful technique for determining temporal variations in the structural properties of biomacromolecules on ultra-short time scales without causing structure damage by employing femtosecond X-ray laser pulses generated by an X-ray free electron laser (XFEL). The mixing rate of reactants and biomolecule samples, as well as the hit rate between crystal samples and x-ray pulses, are critical factors determining TR-SFX performance, such as accurate image acquisition and efficient sample consumption. We here develop two distinct sample delivery systems that enable ultra-fast mixing and on-demand droplet injecting via pneumatic application with a square pulse signal. The first strategy relies on inertial mixing, which is caused by the high-speed collision and subsequent coalescence of droplets ejected through a double nozzle, while the second relies on on-demand pneumatic jetting embedded with a 3D-printed micromixer. First, the colliding behaviors of the droplets ejected through the double nozzle, as well as the inertial mixing within the coalesced droplets, are investigated experimentally and numerically. The mixing performance of the pneumatic jetting system with an integrated micromixer is then evaluated by using similar approaches. The sample delivery system devised in this work is very valuable for three-dimensional biomolecular structure analysis, which is critical for elucidating the mechanisms by which certain proteins cause disease, as well as searching for antibody drugs and new drug candidates.

Luminescence properties of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ red phosphor as the effect of Zn ion (Zn ion의 영향에 따른 $(Y,\;Zn)_2O_3$:$Eu^{3+}$ 적색 형광체의 발광특성)

  • Song, Y.H.;Moon, J.W.;Park, W.J.;Yoon, D.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.6
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    • pp.253-257
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    • 2008
  • To enhance the luminescence properties, the red phosphor composed of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ as doping concentration of Zn ion is synthesized at $1200^{\circ}C$ for 6 hrs in air atmosphere by conventional solid reaction method. As a result of the red phosphor $(Y,\;Zn)_2O_3$:$Eu^{3+}$ is measured X-ray diffraction (XRD), The main peak is nearly corresponded to the same as JCPDS card (No. 41-1105). When the doping concentration of Zn ion is more than 5 mol%, However, the ZnO peak is showed by XRD analysis. Therefore, when the doping concentration of Zn ion is less than 5 mol%, the Zn ion is well mixed in $Y_2O_3$ structure without the impurity phases. The photoluminescence (PL) properties is shown as this phosphor is excited in 254 nm region and the highest emission spectra of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ has shown in 612 nm region because of a typical energy transition ($^5D_0{\rightarrow}^7F_2$) of $Eu^{3+}$ ion. As the doping concentration of Zn ion is more than 10 mol%, the emission peak is suddenly decreased. when the highest emission peak as doping concentration of Zn ion is shown, the composition of this phosphor is $(Y_{0.95},\;Zn_{0.05})_2O_3$:$Eu^{3+}_{0.075}$ and the particle size analyzed by FE-SEM is confirmed from 0.4 to $3{\mu}m$.

Microstructural property and catalytic activity of nano-sized MnOx-CeO2/TiO2 for NH3-SCR (선택적 촉매 환원법 재료로서 나노 사이즈 MnOx-CeO2/TiO2 촉매에 대한 미세 구조적 특성과 촉매활성 평가)

  • Hwang, Sungchul;Jo, Seung-hyeon;Shin, Min-Chul;Cha, Jinseon;Lee, Inwon;Park, Hyun;Lee, Heesoo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.3
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    • pp.115-120
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    • 2016
  • $CeO_2$ is used as a co-catalyst with $TiO_2$ to improve the catalytic activity of $MnO_x$ and characterization of nano-sized powder is identified with de-NOx efficiency. A comparison between $MnO_x-CeO_2/TiO_2$ and single $CeO_2$ was conducted in terms of microstructural analysis to observe the behavior of $CeO_2$ in the ternary catalyst. The $MnO_x-CeO_2/TiO_2$ catalyst was synthesized by sol-gel method and the average particle size of the single $CeO_2$ is about $285{\mu}m$ due to the low thermal stability, whereas the particle size $MnO_x-CeO_2/TiO_2$ is about 130 nm. The strong interaction between Ce and Ti was identified through the EDS mapping by transmission electron microscopy (TEM). The improvement about 20 % of $de-NO_x$ efficiency is observed in the low-temperature ($150^{\circ}C{\sim}250^{\circ}C$) and vigorous oxygen exchange by well-dispersed $CeO_2$ is the reason of catalytic activity improvement.

Ni0.5Zn0.4Cu0.1Fe2O4 Complex Ferrite Nanoparticles Synthesized by Chemical Coprecipitation Predicted by Thermodynamic Modeling

  • Kang, Bo-Sun;Park, Joo-Seok;Ahn, Jong-Pil;Kim, Kwang-Hyun;Tae, Ki-Sik;Lee, Hyun-Ju;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
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    • v.50 no.3
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    • pp.231-237
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    • 2013
  • Thermodynamic modeling of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite system has been adopted as a rational approach to establish routes to better synthesis conditions for pure phase $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite. Quantitative analysis of the different reaction equilibria involved in the precipitation of $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ from aqueous solutions has been used to determine the optimum synthesis conditions. The spinel ferrites, such as magnetite and substitutes for magnetite, with the general formula $MFe_2O_4$, where M= $Fe^{2+}$, $Co^{2+}$, and $Ni^{2+}$ are prepared by coprecipitation of $Fe^{3+}$ and $M^{2+}$ ions with a stoichiometry of $M^{2+}/Fe^{3+}$= 0.5. The average particle size of the as synthesized $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$, measured by transmission electron microscopy (TEM), is 14.2 nm, with a standard deviation of 3.5 nm the size when calculated using X-ray diffraction (XRD) is 16 nm. When $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite is annealed at elevated temperature, larger grains are formed by the necking and mass transport between the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite nanoparticles. Thus, the grain sizes of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ gradually increase as heat treatment temperature increases. Based on the results of Thermogravimetric Analysis (TGA) and Differential Scanning Calorimeter (DSC) analysis, it is found that the hydroxyl groups on the surface of the as synthesized ferrite nanoparticles finally decompose to $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ crystal with heat treatment. The results of XRD and TEM confirmed the nanoscale dimensions and spinel structure of the samples.

Optical and Structural Analysis of BaSi2O2N2:Eu Green Phosphor for High-Color-Rendering Lighting (고연색 백색 광원용 BaSi2O2N2:Eu 형광체의 광학·구조 특성 분석)

  • Lee, Sunghoon;Kang, Taewook;Kang, Hyeonwoo;Jeong, Yongseok;Kim, Jongsu;Heo, Hoon
    • Korean Journal of Materials Research
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    • v.29 no.7
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    • pp.437-442
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    • 2019
  • Green $BaSi_2O_2N_2:0.02Eu^{2+}$ phosphor is synthesized through a two-step solid state reaction method. The first firing is for crystallization, and the second firing is for reduction of $Eu^{3+}$ into $Eu^{2+}$ and growth of crystal grains. By thermal analysis, the three-time endothermic reaction is confirmed: pyrolysis reaction of $BaCO_3$ at $900^{\circ}C$ and phase transitions at $1,300^{\circ}C$ and $1,400^{\circ}C$. By structural analysis, it is confirmed that single phase [$BaSi_2O_2N_2$] is obtained with Cmcm space group of orthorhombic structure. After the first firing the morphology is rod-like type and, after the second firing, the morphology becomes round. Our phosphor shows a green emission with a peak position of 495 nm and a peak width of 32 nm due to the $4f^65d^1{\rightarrow}4f^7$ transition of $Eu^{2+}$ ion. An LED package (chip size $5.6{\times}3.0mm$) is fabricated with a mixture of our green $BaSi_2O_2N_2$, and yellow $Y_3Al_5O_{12}$ and red $Sr_2Si_5N_8$ phosphors. The color rendering index (90) is higher than that of the mixture without our green phosphor (82), which indicates that this is an excellent green candidate for white LEDs with a deluxe color rendering index.

Fabrication and the Electrochemical Characteristics of Petroleum Residue-Based Anode Materials (석유계 잔사유 기반 음극재 제조 및 그 전기화학적 특성)

  • Kim, Daesup;Lim, Chaehun;Kim, Seokjin;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.33 no.5
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    • pp.496-501
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    • 2022
  • In this study, an anode material for lithium secondary batteries was manufactured using petroleum-based residual oil, which is a petroleum refining by-product. Among petroleum-based residual oils, pyrolysis fuel oil (PFO), fluidized catalyst cracking-decant oil (FCC-DO), and vacuum residue (VR) were used as carbon precursors. The physicochemical characteristics of petroleum-based residual oil were confirmed through Matrix-assisted laser desorption/ionization Time-of-Flight (MALDI-TOF) and elemental analysis (EA), and the structural characteristics of anode materials manufactured from residual oil were evaluated using X-ray crystallography (XRD) and Raman spectroscopic techniques. VR was found to contain a wide range of molecular weight distributions and large amounts of impurities compared to PFO and FCC-DO, and PFO and FCC-DO exhibited almost similar physicochemical characteristics. From the XRD analysis results, carbonized PFO and FCC-DO showed similar d002 values. However, it was confirmed that FCC-DO had a more developed layered structure than PFO in Lc (Length of a and c axes in the crystal system) and La values. In addition, FCC-DO showed the best cycle characteristics in electrochemical characteristics evaluation. According to the physicochemical and electrochemical results of the petroleum-based residual oil, FCC-DO is a better carbon precursor for a lithium secondary battery than PFO and VR.

Structural Characteristics and Physical Properties of Wild Silk Fibres; Antheraea pernyi and Antheraea yamamai (야잠사의 구조특성 및 물리적 성질)

  • 권해용;박영환
    • Journal of Sericultural and Entomological Science
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    • v.36 no.2
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    • pp.138-146
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    • 1994
  • The structural characteristics of Antheraea yamamai and Antheraea pernyi silk were investigated by using x-ray diffraction method, IR spectroscopy and polarizing microscopy. The amino acid composition, fiber density, thermal decomposition temperature and glass transition temperature were also measured for relating these physical properties to the structure in comparison with those of Bombyx mori silk fiber. There was no significant structural difference between A. yamamai and A. pernyi silk fiber on an examination of x-ray diffraction curve and IR spectrum. Both of these wild silk fibers showed double diffraction peaks at the Bragg angle 2Θ16.7˚ and 20.5˚by x-ray diffraction analysis as well as IR absorption peaks for the bending vibration of specific groups related to ala-ala amino acid sequence. On the other hand, the x-ray diffraction curve and IR spectrum of Bombyx mori silk fiber are different from those of wild silk fibers, indicating different crystal structure as well as amino acid sequences. It showed under the polarizing microscope examination that the birefringence and optical orientation factor of wild silk fibers are much lower than those of B. mori silk. Also, the surface of degummed wild silk fibers was characterized by the longitudinal stripes of microfibrils in the direction of fiber axies. The amino acid composition, which is strongly related to the fine structure and properties, was not significantly different between these two wild silk fibers. However, the alanine content was somewhat less and polar amino acid content more for A. yamamai. As a result of fiber density measurement, the specific gravities of B. mori, A. pernyi and A. yamamai were 1.355~1.356, 1.308~1.311, 1.265~1.301g/㎤ in the order, respectively. The calculated crystallinity(%) was 64% for B. mori and 51~52% for wild silk fibers, which showed same trend by IR method in spite of somewhat higher value. The thermal decomposition behaviour was examined by DSC and TGA, showing that the degradation temperature was in the order of B mori, A. prernyi and A. yamamai at around 350$^{\circ}C$. It was also observed by TGA that the decomposition seems to proceed step by step according to their specific regions in the fiber structure, resulting the difference in their thermal stabilities. The glass transition temperature was turned out to be 220$^{\circ}C$ for B. mori, 240$^{\circ}C$ A. yamamai and 255$^{\circ}C$ A. pernyi by the dynamic mechanical analysis. It is expected that the chemical properties are affected by the dynamic mechanical behavior in accordance with their structural characters.

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SINUS FLOOR GRAFTING USING CALCIUM PHOSPHATE NANO-CRYSTAL COATED XENOGENIC BONE AND AUTOLOGOUS BONE (칼슘포스페이트 나노-크리스탈이 코팅된 골이식재와 자가골을 병행 이용한 상악동 거상술)

  • Pang, Kang-Mi;Li, Bo-Han;Alrashidan, Mohamed;Yoo, Sang-Bae;Sung, Mi-Ae;Kim, Soung-Min;Jahng, Jeong-Won;Kim, Myung-Jin;Ko, Jea-Seung;Lee, Jong-Ho
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.31 no.3
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    • pp.243-248
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    • 2009
  • Purpose: Rehabilitation of the edentulous posterior maxilla with dental implants often poses difficulty because of insufficient bone volume caused by pneumatization of the maxillary sinus and by crestal bone resorption. Sinus grafting technique was developed to increase the vertical height to overcome this problem. The present study was designed to evaluate the sinus floor augmentation with anorganic bovine bone (Bio-$cera^{TM}$) using histomorphometric and clinical measures. Patients and methods: Thirteen patients were involved in this study and underwent total 14 sinus lift procedures. Residual bone height was ${\geq}2mm$ and ${\leq}6mm$. Lateral window approach was used, with grafting using Bio-$cera^{TM}$ only(n=1) or mixed with autogenous bone from ramus and/or maxillary tuberosity(n=13). After 6 months of healing, implant sites were created with 3mm diameter trephine and biopsies taken for histomorphometric analysis. The parameters assessed were area fraction of new bone, graft material and connective tissue. Immediate and 6 months after grafting surgery, and 6 months after implantation, computed tomography (CT) was taken and the sinus graft was evaluated morphometric analysis. After implant installation at the grafted area, the clinical outcome was checked. Results: Histomorphometry was done in ten patients.Bio-$cera^{TM}$ particles were surrounded by newly formed bone. The graft particles and newly formed bone were surrounded by connective tissue including small capillaries in some fields. Imaging processing revealed $24.86{\pm}7.59%$ of new bone, $38.20{\pm}13.19%$ connective tissue, and $36.92{\pm}14.51%$ of remaining Bio-$cera^{TM}$ particles. All grafted sites received an implant, and in all cases sufficient bone height was achieved to install implants. The increase in ridge height was about $15.9{\pm}1.8mm$ immediately after operation (from 13mm to 19mm). After 6 months operation, ridge height was reduced about $11.5{\pm}13.5%$. After implant installation, average marginal bone loss after 6 months was $0.3{\pm}0.15mm$. Conclusion: Bio-$cera^{TM}$ showed new bone formation similar with Bio-$Oss^{(R)}$ histomorphometrically and appeared to be an effective bone substitute in maxillary sinus augmentation procedure with the residual bone height from 2 to 6mm.