• 제목/요약/키워드: X-ray structure analysis

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수침이 도토리 앙금의 호화에 미치는 영향 (Effects of Soaking on Pasting Gelatinization of Acorn Flour)

  • 나환식;오금순;박종훈;김관;김성곤
    • 한국식품영양과학회지
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    • 제29권5호
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    • pp.770-776
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    • 2000
  • Pasting gelatinization of acorn flours which were prepared with soaked nut and sediment at 7.8$^{\circ}C$ for 0, 1, 2, 3 and 4 days were investigated. The peak temperature of gelatinization of untreated acorn flour (0-0) by Rapid Visco Analyzer was 73.1$^{\circ}C$, respectively, but those of flours were decreased by soaking. Peak viscosity, setback and breakdown of acorn flours were increased by soaking. In addition, consistency was increased by soaking treatment. From the result of the pasting properties, gel formation ability of acorn flour was increased with increasing soaking days of acorn nut and soaking times of sediment. The gelatinization temperature examined by X-ray diffractometry was lowered with increasing of soaking days. The observation of microstructure through a scanning electron microscope revealed that gelatinized acorn flour showed loser their original shape and structure than that of with out soaking treatment (0-0). The degree of gelatinization under the fixed temperature increased with increasing soaking days. From these results, it might be concluded that the increase of soaking days and soaking times is the factor affecting the gelatinization of acorn flour.

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Preparation and Electrical Properties of Manganese-incorporated Neodymium Oxide System

  • Jong Sik Park;Keu Hong Kim;Chul Hyun Yo;Sung Han Lee
    • Bulletin of the Korean Chemical Society
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    • 제15권9호
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    • pp.713-718
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    • 1994
  • Manganese-incorporated neodymium oxide systems with a variety of Mn mol% were prepared to investigate the effect of doping on the electrical properties of neodymium oxide. XRD, XPS, SEM, DSC, and TG techniques were used to analyze the specimens. The systems containing 2, 5, 8, and 10 mol% Mn were found to be solid solutions by X-ray diffraction analysis and the lattice parameters were obtained for the single-phase hexagonal structure by the Nelson-Riley method. The lattice parameters, a and c, decreased with increasing Mn mol%. Scanning electron photomicrographs of the specimens showed that the grain size decreased with increasing Mn mol%. The curves of log conductivity plotted as a function of 1/T in the temperature range from 500 to 1000$^{\circ}C$ at $PO_2$'s of $10^{-5}$ to $10^{-1}$ atm for the specimens were divided into high-and low-temperature regions with inflection points near 820-890$^{\circ}C$. The activation energies obtained from the slopes were 0.53-0.87 eV for low-temperature region and 1.40-1.91 eV for high-temperature region. The electrical conductivities increased with increasing Mn mol% and $PO_2$, indicating that all the specimens were p-type semiconductors. At $PO_2$'s below $10^{-3}$ atm, the electrical conductivity was affected by the chemisorption of oxygen molecule in the temperature range of 660 to 850$^{\circ}C$. It is suggested that electron holes generated by oxygen incorporation into the oxide are charge carriers for the electrical conduction in the high-temperature region and the system includes ionic conduction owing to the diffusion of oxygen atoms in the low-temperature region.

Superhard SiC Thin Films with a Microstructure of Nanocolumnar Crystalline Grains and an Amorphous Intergranular Phase

  • Lim, Kwan-Won;Sim, Yong-Sub;Huh, Joo-Youl;Park, Jong-Keuk;Lee, Wook-Seong;Baik, Young-Joon
    • Corrosion Science and Technology
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    • 제18권5호
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    • pp.206-211
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    • 2019
  • Silicon carbide (SiC) thin films become superhard when they have microstructures of nanocolumnar crystalline grains (NCCG) with an intergranular amorphous SiC matrix. We investigated the role of ion bombardment and deposition temperature in forming the NCCG in SiC thin films. A direct-current (DC) unbalanced magnetron sputtering method was used with pure Ar as sputtering gas to deposit the SiC thin films at fixed target power of 200 W and chamber pressure of 0.4 Pa. The Ar ion bombardment of the deposited films was conducted by applying a negative DC bias voltage 0-100 V to the substrate during deposition. The deposition temperature was varied between room temperature and $450^{\circ}C$. Above a critical bias voltage of -80 V, the NCCG formed, whereas, below it, the SiC films were amorphous. Additionally, a minimum thermal energy (corresponding to a deposition temperature of $450^{\circ}C$ in this study) was required for the NCCG formation. Transmission electron microscopy, Raman spectroscopy, and glancing angle X-ray diffraction analysis (GAXRD) were conducted to probe the samples' structural characteristics. Of those methods, Raman spectroscopy was a particularly efficient non-destructive tool to analyze the formation of the SiC NCCG in the film, whereas GAXRD was insufficiently sensitive.

금속산화물 분말의 동결건조 및 수소환원에 의한 Mo-Cu 다공체 제조 (Fabrication of Porous Mo-Cu by Freeze Drying and Hydrogen Reduction of Metal Oxide Powders)

  • 강현지;한주연;오승탁
    • 한국분말재료학회지
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    • 제26권1호
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    • pp.1-5
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    • 2019
  • In this study, porous Mo-5 wt% Cu with unidirectionally aligned pores is prepared by freeze drying of camphene slurry with $MoO_3-CuO$ powders. Unidirectional freezing of camphene slurry with dispersion stability is conducted at $-25^{\circ}C$, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The green bodies are hydrogen-reduced at $750^{\circ}C$ and sintered at $1000^{\circ}C$ for 1 h. X-ray diffraction analysis reveals that $MoO_3-CuO$ composite powders are completely converted to a Mo-and-Cu phase without any reaction phases by hydrogen reduction. The sintered bodies with the Mo-Cu phase show large and aligned parallel pores to the camphene growth direction as well as small pores in the internal walls of large pores. The pore size and porosity decrease with increasing composite powder content from 5 to 10 vol%. The change of pore characteristics is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

석탄 비산재로부터 저알칼리 조건에서 합성된 Na-A 제올라이트의 Sr, Cs 및 Na 이온의 흡탈착 특성 (Adsorption and Desorption Characteristics of Sr, Cs, and Na Ions with Na-A Zeolite Synthesized from Coal Fly Ash in Low-Alkali Condition)

  • 최정학;이창한
    • 한국환경과학회지
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    • 제28권6호
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    • pp.561-570
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    • 2019
  • A zeolitic material (Z-Y2) was synthesized from Coal Fly Ash (CFA) using a fusion/hydrothermal method under low-alkali condition (NaOH/CFA = 0.6). The adsorption performance of the prepared zeolite was evaluated by monitoring its removal efficiencies for Sr and Cs ions, which are well-known as significant radionuclides in liquid radioactive waste. The XRD (X-ray diffraction) patterns of the synthesized Z-Y2 indicated that a Na-A type zeolite was formed from raw coal fly ash. The SEM (scanning electron microscope) images also showed that a cubic crystal structure of size $1{\sim}3{\mu}m$ was formed on its surface. In the adsorption kinetic analysis, the adsorption of Sr and Cs ions on Z-Y2 fitted the pseudo-second-order kinetic model well, instead of the pseudo-first-order kinetic model. The second-order kinetic rate constant ($k_2$) was determined to be $0.0614g/mmol{\cdot}min$ for Sr and $1.8172g/mmol{\cdot}min$ for Cs. The adsorption equilibria of Sr and Cs ions on Z-Y2 were fitted successfully by Langmuir model. The maximum adsorption capacity ($q_m$) of Sr and Cs was calculated as 1.6846 mmol/g and 1.2055 mmol/g, respectively. The maximum desorption capacity ($q_{dm}$) of the Na ions estimated via the Langmuir desorption model was 2.4196 mmol/g for Sr and 2.1870 mmol/g for Cs. The molar ratio of the desorption/adsorption capacity ($q_{dm}/q_m$) was determined to be 1.44 for Na/Sr and 1.81 for Na/Cs, indicating that the amounts of desorbed Na ions and adsorbed Sr and Cs ions did not yield an equimolar ratio when using Z-Y2.

고분자 전해질 연료전지용 술폰화된 폴리(아릴렌 이써 설폰)/SPVdF-co-HFP 브렌딩 멤브레인의 제조 및 특성 분석 (Preparation and Characterization of SPAES/SPVdF-co-HFP Blending Membranes for Polymer Electrolyte Membrane Fuel Cells)

  • 박철진;김애란;유동진
    • 한국수소및신에너지학회논문집
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    • 제30권3호
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    • pp.227-236
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    • 2019
  • In this work, preparation and characterizations of hybrid membranes containing sulfonated poly(arylene ether sulfone) (SPES) and sulfonated poly(vinylidene fluoride-co-hexafluoropropylene) (SPVdF-co-HFP) (20, 30 or 40 wt%) were carried out. The structure of hybrid membranes was confirmed using X-ray diffraction (XRD) analysis and the Fourier transform infrared (FT-IR) spectroscopy. The prepared SPAES/SPVdF-30 membrane exhibits higher ionic conductivity of 68.9 mS/cm at $90^{\circ}C$ and 100% RH. Besides, the other studies showed that the hybrid membrane has good oxidation stability, thermal stability, and mechanical stability. Thus, we believe that the prepared hybrid membrane is suitable for the development of membranes for fuel cell applications.

Preparation and Characterization of Ordered Perovskite (CaLa) (MgMo) $_6$

  • Choy, Jin-Ho;Hong, Seung-Tae;Suh, Hyeong-Mi
    • Bulletin of the Korean Chemical Society
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    • 제9권6호
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    • pp.345-349
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    • 1988
  • The polycrystalline powder of (CaLa) (MgMo)$O_6$ has been prepared at $1350^{\circ}C$ in $H_2/H_2O$ and $N_2$ flowing atmosphere. The powder X-ray diffraction pattern indicates that (CaLa) (MgMo)$O_6$ has a monoclinic perovskite structure with the lattice constants $a_0=b_0=7.901(1){\AA}$, $c =7.875(1){\AA}\;and\;{\gamma}=89^{\circ}$16'(1'), which can be reduced to orthorhombic unit cell, a = 5.551(1) ${\AA}$, b = 5.622(1) ${\AA}$ and c = 7.875(1) ${\AA}$. The infrared spectrum shows two strong absorption bands with their maxima at 590($ν_3$) and 380($ν_4$) cm, which are attributed to $2T_{1u}$ modes indicating the existence of highly charged molybdenum octahedron $MoO_6$ in the crystal lattice. According to the magnetic susceptibility measurement, the compound follows the Curie-Weiss law below room temperature with the effective magnetic moment 1.83(1)$_{{\mu}B}$, which is well consistent with that of spin only value (1.73 $_{\mu}_B$) for $Mo^{5+}$ with $4d^1$-electronic configuration within the limit of experimental error. From the thermogravimetric analysis, it has been confirmed that (CaLa) (MgMo)$O_6$ decomposes gradually into $CaMoO_4,\;MoO_3,\;MgO,\;La_2O_3$ and unidentified phases due to the oxidation of $Mo^{5+}$ to $Mo^{6+}$.

Surface characteristics and bioactivity of minocycline-treated Ti-6Al-4V alloy

  • Lee, Jung-Hyuk;Sun, Young-Gon;Na, Eui-Ri;Moon, Jong-Wook;Kim, Young-Joon
    • 구강생물연구
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    • 제42권4호
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    • pp.187-197
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    • 2018
  • Chemical agents such as minocycline (MC) and citric acid (CA) were suggested in the treatment of contaminated implant surface. In this study, MC-HCl treatment was performed to enhance surface characteristics of titanium alloy surface. The purpose of this study was to assess the characteristics and the biocompatibility of Ti-6Al-4V surface treated by MC. Alpha-beta titanium alloy (Ti-6Al-4V) samples were prepared and they were divided into 6 groups according to chemical concentration and treatment time. These groups include 1) group I, non-treated smooth titanium alloy; 2) group II, MC 1.5 mg/mL for 1 hour; 3) group III, MC 1.5 mg/mL for 24 hours; 4) group IV, MC 15 mg/mL for 10 minutes; 5) group V, MC 100 mg/mL for 5 minutes; 6) group VI, pH1 CA for 3 minutes. The analysis of the surface characteristics of MC-treated titanium alloy was executed using scanning electron microscopy, roughness test, and X-ray photoelectron spectroscopy (XPS). Cell adhesion and MTT assay was done using MC3T3 cell. Titanium surfaces treated with MC indicated a more smoothened surface microstructure. For group II and III, the new peaks of rutile TiO2 were found. Group II and V have more basic group of Ti-OH form in XPS. In MTT assay, all MC-treated groups showed significantly higher cell viability compared to control. The surface roughness, crystal structure, surface hydrophilicity, cell viability of smooth titanium surface was improved by MC treatment. Compared with the control experiment and CA-treated group, smooth titanium surface treated with MC showed improved surface characteristics and cell biocompatibility.

Optimization red emission of SrMoO4: Eu3+ via hydro-thermal co-precipitation synthesis using orthogonal experiment

  • Tan, Yongjun;Luo, Xuedan;Mao, Mingfu;Shu, Dehua;Shan, Wenfei;Li, Guizhi;Guo, Dongcai
    • Current Applied Physics
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    • 제18권11호
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    • pp.1403-1409
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    • 2018
  • In the present study, the $SrMoO_4:Eu^{3+}$ phosphors has been synthesized through hydro-thermal co-precipitation method, and single factor and orthogonal experiment method was adopted to find optimal synthesis condition. It is interesting to note that hydro-thermal temperature is a prominent effect on the luminescent intensity of $SrMoO_4:Eu^{3+}$ red phosphor, followed by co-precipitation temperature, calcining time, and the doping amount of $Eu^{3+}$. The optimal synthesis conditions were obtained: hydro-thermal temperature is $145^{\circ}C$, co-precipitation temperature is $35^{\circ}C$, the calcining time is 2.5 h, and the doping amount of activator $Eu^{3+}$ is 25%. Subsequently, the crystalline particle size, phase composition and morphology of the synthesized phosphors were evaluated by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The results show that these phosphors possess a scheelite-type tetragonal structure, and the particle size is about $0.2{\mu}m$. Spectroscopic investigations of the synthesized phosphors are carried out with the help of photo-luminescence excitation and emission analysis. The studies reveal that $SrMoO_4:Eu^{3+}$ phosphor efficiently convert radiation of 394 nm-592 and 616 nm for red light, and the luminescence intensity of $SrMoO_4:Eu^{3+}$ phosphors is improved. $SrMoO_4:Eu^{3+}$ phosphors may be a potential application for enhancing the efficiency of white LEDs.

WO3/tert-butyl alcohol 슬러리의 동결건조 조건이 다공체의 미세구조 특성에 미치는 영향 (Effect of Freeze Drying Condition of WO3/Tert-Butyl Alcohol Slurry on the Microstructural Characteristics of Porous Body)

  • 이의선;허연지;석명진;오승탁
    • 한국분말재료학회지
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    • 제28권4호
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    • pp.331-335
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    • 2021
  • The effects of drying temperature on the microstructure of porous W fabricated by the freeze-casting process of tert-butyl alcohol slurry with WO3 powder was investigated. Green bodies were hydrogen-reduced at 800℃ for 1 h and sintered at 1000℃ for 6 h. X-ray diffraction analysis revealed that WO3 powders were completely converted to W without any reaction phases by hydrogen reduction. The sintered body showed pores aligned in the direction of tert-butyl alcohol growth, and the porosity and pore size decreased as the amount of WO3 increased from 5 to 10vol%. As the drying temperature of the frozen body increased from -25℃ to -10℃, the pore size and thickness of the struts increased. The change in microstructural characteristics based on the amount of powder added and the drying temperature was explained by the growth behavior of the freezing agent and the degree of rearrangement of the solid powder during the solidification of the slurry.