• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.564-573
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• 2022

Calcium carbonate (CaCO₃) exhibits three polymorphs: calcite with arhombohedral, vaterite with a spherical, and aragonite with a needle-like structure. Qualitative and quantitative analyses of the morphology of CaCO₃ are very important to investigate the synthesis of single-crystal vaterite and aragonite. In this work, the polymorphs of calcium carbonate were quantitatively analyzed using XRD. Pure vaterite and pure aragonite were synthesized and the peak distribution of a single phase was analyzed. The vaterite fraction of a mixture of calcite and vaterite was calculated based on the intensity of a specific diffraction peak, and compared to the results based on the peak area. The mean value of f_sV (the correction factor for the peak area of vaterite) was 0.654. The phase analysis of calcite-aragonite mixtures was performed, and the mean value of f_sA (the correction factor for the peak area of aragonite) was obtained as 0.6713. Using these factors, Eq. (24)~Eq. (32) for the quantitative analysis based on the total peak area of XRD were derived to calculate the phase contents of ternary phase CaCO₃. And three-component XRD section was defined considering overlapping sections.

• Journal of the Korean Vacuum Society
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• v.19 no.1
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• pp.52-57
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• 2010

$BiFeO_3/Pb(Zr_{0.52}Ti_{0.48})O_3$(BFO/PZT) multilayer thin films have been prepared on a Pt/Ti/$SiO_2$/Si(100) substrate by chemical solution deposition. BFO single layer, BFO/PZT bilayer and multilayer thin films were studied for comparison. X-ray diffraction analysis showed that the crystal structure of all films was multi-orientated perovskite phase without amorphous and impurity phase. The leakage current density at 500 kV/cm was reduced by approximately four and five orders of magnitude by bilayer and multilayer structure films, compared with BFO single layer film. The low leakage current density leads to saturated P-E hysteresis loops of bilayer and multilayer films. In BFO/PZT multlayer film, saturated remanent polarization of $44.3{\mu}C/cm^2$ was obtained at room temperature at 1 kHz with the coercive field($2E_c$) of 681.4 kV/cm.

• 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.

• 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.

• 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.

• 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 $3{\mu}m$.

• 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.

• 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.

• 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.

• 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.