• Title/Summary/Keyword: X-ray crystal diffraction

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Crystallograpbic and Magnetic Properties of $Ni_{0.65}Zn_{0.35}Cu_{0.3}Fe_{1.7}O_4$ ($Ni_{0.65}Zn_{0.35}Cu_{0.3}Fe_{1.7}O_4$의 결정학적 및 자기적 특성 연구)

  • 김우철;김삼진;김철성;이승화
    • Journal of the Korean Magnetics Society
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    • v.9 no.3
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    • pp.136-142
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    • 1999
  • $Ni_{0.65}Zn_{0.35}Cu_{0.3}Fe_{1.7}O_4$ has been studied with x-ray diffraction, Mossbauer spectroscopy, and vibrating sample magnetometer. The crystal structure is found to be a cubic spinel with the lattice constant $a_0=8.403{\AA}$. Mossbauer spectra of have been taken at various temperatures ranging from 12 K to 665 K. as the temperature increases toward $T_N$ a systematic line broadening effect in the Mossbauer spectrum is observed and interpreted to originate from different temperature dependencies of the magenetic hyperfine fields at various iron sites. Also, by using binomial distribution equation we obtained the hyperfine fields of tetrahedral[A] and octahedral sites[B], $H_{hf}(A)=470\;kOe,\; H_{hf}(B0)=495 \;kOe,\; H_{hf}(B1)=485\;kOe, \;H_{hf}(B2)=453\;kOe,\; H_{hf}(B3)=424\;kOe,\; H_{hf}(B4)=390\;kOe,\; H_{hf}(Bavr)=451\;kOe$ respectively at room temperature. The isomer shift indicates that the iron ions are ferric at tetrahedral[A] and octahedral sites[B], respectively. The Neel temperature is determined to be $T_N=665\;K$. The results of the VSM data gave the magnetic moment and coercivity values of $M_S=66\; emu/g\;and\;H_C=36\;Oe$.

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Synthesis and Characterization of Polymers with Azobenzene and Hexamethylene Groups in Main Chain (주사슬에 아조벤젠기와 헥사메틸렌기를 갖는 고분자의 합성 및 특성)

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.86-92
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    • 2019
  • Polymers with various compositions of azobenzene and hexamethylene groups in the main chain were synthesized by a Schotten-Baumann reaction and their properties were investigated. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and x-ray diffraction. The polymers showed an inherent viscosity of 1.28-1.36 dl/g and were relatively insoluble in most organic solvents. The melt transition temperature increased rapidly with increasing number of azobenzene groups in the polymer. When the azobenzene monomer content was more than 50 mol%, no melting transition occurred below the decomposition temperature. Among the polymers with a melt transition temperature, the MP-A3C7 and MP-A5C5 polymers were liquid crystalline materials and exhibited a nematic phase with weak liquid crystallinity over a wide liquid crystal temperature range. This difference in the properties of the synthesized polymers is likely due to the changes in intermolecular forces resulting from the linearity and polarity of the trans-form of azobenzene.

Size Control and Dispersion Properties of Illite Clay by Physicochemical Treatment (물리화학적 처리에 의한 일라이트 점토광물의 입도조절 및 분산특성)

  • Lim, Jae Won;Jeong, Euigyung;Seo, Kyeong-won;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.22 no.2
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    • pp.133-137
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    • 2011
  • In this study, illite was size-reduced using a wet-ball-milling treatment to improve its dispersion. Changes in illite particle size, size distribution, and dispersion characteristics after varying the treatment period were investigated. And the dispersion and dispersion stability of illite solution after 2 h wet ball milling treatment with different pH conditions were also evaluated. The illite particle size significantly decreased as the treatment time increased and the size reduction effect of wet ball milling deteriorated above 2 h treatment time. In addition, illite particle size was more evenly distributed as the treatment time increased. X-ray diffraction (XRD) analysis showed that no crystal structural changes of illite were induced, but the characteristic peak of illite the weaker due to the size reduction and exfoliation, as the treatment time increased. Zeta potential analysis showed that the illite dispersion improved, as the treatment time increased. The illite wet-ball-mill treated at pH 2 had the lowest dispersion stability. Illite dispersion and dispersion stability increased as pH increased, due to the increase in surface ionization. Hence, the results showed that as the treatment time increased, the illite particle size decreased, and dispersion and dispersion stability improved due to the increase in surface energy and repulsion force between particles.

Synthesis and Characterization of Zeolite Using Water Treatment Sludge (정수슬러지를 이용한 제올라이트의 합성 및 특성연구)

  • Ko, Hyun Jin;Ko, Yong Sig
    • Clean Technology
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    • v.26 no.4
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    • pp.263-269
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    • 2020
  • Zeolite was synthesized hydrothermally using the water-treatment sludge, and the effects of various synthesis parameters like reaction temperature, reaction time, and Na2O/SiO2 molar ratio on the crystallization of zeolite were investigated. Crystal structure, physical property, and thermal stability of zeolite crystals were characterized by X-ray powder diffraction, FTIR spectroscopy, BET nitrogen adsorption, and TGA measurements. The removal efficiencies of nitrogen in ammonia, heavy metal ions, and TOC were calculated to evaluate zeolite's adsorption capacity. The primary chemical composition of water-treatment sludge was 28.79% Al2O3 and 27.06% SiO2. The zeolites were synthesized by merely employing the water-treatment sludge as silica and alumina sources without additional chemicals. Zeolite crystals synthesized through the water-treatment sludge were confirmed as an A-type zeolite structure. Zeolite A had the highest crystallinity obtained from a gel with the molar composition 2.1Na2O-Al2O3-1.6SiO2-65H2O after 5 h at a temperature of 90 ℃. The specific surface area of zeolite obtained was 55 ㎡ g-1, which was higher than commercial zeolite A. The removal efficiency of nitrogen in ammonia was 68% after 3 h of reaction time, while the removal efficiencies of Pb2+ and Cd2+ ions were 99.1% and 99.3%, respectively. These results indicate active ion exchange between Pb2+ or Cd2+ ion and Na+ ion in the zeolite framework. The adsorption experiments on the different zeolite addition conditions were performed for 3 h with 300 ppm humic acid. Based on the results, TOC's highest efficiency was 83% when 5 g of zeolite was added.

Redispersion of Sintered PtSn Catalyst by Oxygen Treatment (소결된 백금주석 촉매의 산소 처리에 의한 재분산 연구)

  • Choi, Yi Sun;Kim, Tae hee;Koh, Hyoung Lim
    • Korean Chemical Engineering Research
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    • v.60 no.3
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    • pp.459-467
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    • 2022
  • Redispersion of Pt-Sn particles in Pt, PtSn catalyst which have been sintered by high temperature hydrogen reduction was investigated using oxygen treatment with various temperatures. The aim of this study was to understand the relationship between the catalytic activity for propane dehydrogenation reaction and the change in the physicochemical properties of the catalyst. X-ray diffraction analysis (XRD), CO pulse chemisorption, and H2 temperature programmed reduction (H2-TPR) were performed to investigate the state of active metal and interactions between particles of redispersed catalyst. It was confirmed that the dispersion and particle size of platinum, the crystal phase of the catalyst, and the reduction behavior were changed according to the oxygen treatment. As for the catalytic activity in propane dehydrogeantion, sintered PtSn catalyst treated with oxygen at 500 ℃ showed best activity and recovery of initial activity. It was confirm that catalyst after oxygen treatment at 500 ℃ showed high dispersion of Pt and decreased particle size as the results of CO pulse chemisorption and XRD of catalyst, and thus the redispersion of PtSn particles in sintered catalyst was occurred. Catalytic activity was recovered due to redispersion using oxygen treatment, and the activity recovery of the PtSn catalyst was higher than that of Pt catalyst.

A study on the preparation and analysis of cordierite by sol-gel method (졸-겔법에 의한 코디어라이트 제조와 분석에 관한 연구)

  • Chun, Kyung Soo;Lee, Young Hwan
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.123-128
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    • 2008
  • The golden turbid solution of cordierite precursor was obtained by using magnesium ethoxide in sol-gel method, while the clear solution of cordierite precursor was obtained when 5%-$Zr(OC_3H_7)_4$ solution was used in the sol-gel reaction. $SiO_2$ component was confirmed by infrared spectra showing $1045cm^{-1}$ and the stretching vibration of gelish $SiO_4$ showed $1140cm^{-1}$ and $940cm^{-1}$. The component of $Al_2O_3$ showed at $580cm^{-1}$ and network structure of $Al_2O_6$ showed at $680cm^{-1}$. The component of MgO was confirmed at $575cm^{-1}$ as the stretching vibration. X-ray diffraction analysis showed ${\mu}$-cordierite crystal was showed up at temperature above $1000^{\circ}C$ at the mole ratio of cordierite precursor and water (1:5). ${\mu}$-Cordierite and ${\alpha}$-cordierite were coexisted at $1050^{\circ}C$ for the mole ratio of cordierite precursor and ammonia (1:5) while ${\alpha}$-cordierite was only existed at $1100^{\circ}C$ for the same mole ratio as mentioned above.

Physicochemical Properties of Cross-linked Waxy Rice Starches and Its Application to Yukwa (가교화 찹쌀전분의 물리화학적 성질 및 유과제조 특성)

  • Yu, Chul;Choi, Hyun-Wook;Kim, Chong-Tai;Ahn, Soon-Cheol;Choi, Sung-Won;Kim, Byung-Yong;Baik, Moo-Yeol
    • Korean Journal of Food Science and Technology
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    • v.39 no.5
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    • pp.534-540
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    • 2007
  • In this study, waxy rice starch was chemically modified using phosphorous oxychloride ($POCl_3$, 0.002-0.008%). Then the physicochemical properties of resulting cross-linked waxy rice starches were investigated in order to reduce the steeping time of Yukwa (a Korean oil-puffed rice snack) processing. The swelling powers of the cross-linked waxy rice starch samples were higher than the native waxy rice starch at temperatures above $60^{\circ}C$, and their increases were proportional to the $POCl_3$, concentration. The solubility of the cross-linked waxy rice starch was lower (1.6-3.4%) than the native waxy rice starch (2.7-6.1%). However, the moisture sorption isotherm of the cross-linked waxy rice starch was not significantly different from the native waxy rice starch. The rapid visco analyze. (RVA) pasting temperatures $(65.4-67^{\circ}C)$ of the cross-linked waxy rice starch were lower than those of the native starch $(67^{\circ}C)$. The RVA peak viscosities (287-337 RVU) of the cross-linked waxy rice starch were higher than that of native starch (179 rapid visco units (RVU)), and increased with increasing $POCl_3$ concentration. For the differential scornning calorimeter thermal characteristics, although Tc shifted toward higher temperatures with cross-linking, the To, Tp, and amylopectiin melting enthalpy of the cross-linked waxy rice starch showed no differences compared to the native waxy rice starch. The X-ray diffraction patterns of both the native and cross-linked waxy rice starches showed typical A-type crystal patterns, suggesting that cross-linking mainly occurs in the amorphous regions of starch granules. Therefore, the cross-linking reaction did not change the crystalline region, but altered the amorphous region of the waxy rice starch molecules, resulting in changes of solubility and RVA pasting properties in the cross-linked waxy rice starch. In summary, since cross-linked waxy rice starch has a high puffing efficiency and no browning reaction, it may be applicable for Yukwa processing without a long steeping process.

Synthesis and Electrochemical Properties of Carbon Coated Li4Ti5O12 using PVC (PVC를 원료로 탄소코팅한 Li4Ti5O12의 합성 및 전기화학적 특성)

  • Hyun, Si-Cheol;Na, Byung-Ki
    • Clean Technology
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    • v.24 no.1
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    • pp.77-84
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    • 2018
  • In this study, $Li_4Ti_5O_{12}$ anode materials for lithium ion battery were synthesized by dry ball-mill method. Polyvinyl chloride (PVC) as a carbon source was added to improve electrochemical properties. When the PVC was added after $Li_4Ti_5O_{12}$ formation, the spinel structure was well synthesized and it was confirmed by X-ray diffraction (XRD) experiments. When the carbon material was added before the synthesis and the heat treatment was performed, it was confirmed that a material having a different crystal structure was synthesized even when a small amount of carbon material was added. In the case of $Li_4Ti_5O_{12}$ without the carbon material, the electrical conductivity value was about $10{\mu}S\;m^{-1}$, which was very small and similar to that of the nonconductor. As the carbon was added, the electrical conductivity was greatly improved and increased up to 10,000 times. Electrochemical impedance spectroscopy (EIS) analysis showed that the size of semicircle corresponding to the resistance decreased with the carbon addition. This indicates that the resistance inside the electrode is reduced. According to the Cyclic voltammetry (CV) analysis, the potential difference between the oxidation peak and the reduction peak was reduced with carbon addition. This means that the rate of lithium ion insertion and deinsertion was increased. $Li_4Ti_5O_{12}$ with 9.5 wt% PVC added sample showed the best properties in rate capabilities of $180mA\;h\;g^{-1}$ at 0.2 C-rate, $165mA\;h\;g^{-1}$ at 0.5 C-rate, and $95.8mA\;h\;g^{-1}$ at 5 C-rate.

Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

Fabrication and characteristics of modified PZT System doped With $La_2O_3$ ($La_2O_3$가 첨가된 modified PZT계의 제조 및 특성)

  • 황학인;박준식;오근호
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.418-427
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    • 1997
  • The effect of $La_2O_3$ as a dopant on the microstructure structure, crystal structure and electrical properties was studied. $0.05Pb(Sn_{0.5}Sb_{0.5})O_3+0.11PbTiO_3+0.84PbZroO_3+0.4Wt%MnO_2$ (=0.05PSS +0.11PT+0.84PZ+0.4wt%$MnO_2$) systems doped with 0, 0.1, 0.3, 0.5, 0.7, 1, 3, 5 mole% $La_2O_3$ were fabricated and investigated sintering density, crystal structure and micro-structure. The sintered 0.05PSS+0.11PT+0.84PZ+0.4wt%$MnO_2$ system doped with $La_2O_3$showed sintering density of the range of 7.683 g/㎤ of 0 mole% doping to 7.815 g/㎤ of 0 mole% doping. The average grain sizes in the range of 0 to 5 mole% $La_2O_3$were decreased from 9.0 $\mu\textrm{m}$ to 1.3 $\mu\textrm{m}$. X-ray diffraction investigation of sintered bodies showed that solid solutions were formed between 0.05PSS+0.11PT+0.84PZ+0.4wt%$MnO_2$ system and $La_2O_3$ in the range of 0 to 1 mole% but second phases were formed in case of 3, 5 mole%. Dielectric constants at 1 kHz were increased with 0 to 3 mlole% $La_2O_3$ before and after poling at the condition of 5 $KV_{DC}$/mm at $120^{\circ}C$ or $140^{\circ}C$ during 20 minutes. All Dielectric losses at 1 kHz were less than 1%, Curie temperatures were $208^{\circ}C$, $183^{\circ}C$, $152^{\circ}C$ and $127^{\circ}C$ at 0, 0.5, 1, 3 mole% $La_2O_3$ respectively. The values of $K_p$ were increased from 0 to 3 mole% $La_2O_3$ after poling at condition of 5 $KV_{DC}$mm at the condition of $120^{\circ}C$ or $140^{\circ}C$. The case of 0.7 mole% $La_2O_3$doped 0.05PSS+0.11PT+0.84PZ+0.4wt%$MnO_2$ system showed $K_p$ of 14.5% by poling at $140^{\circ}C$ during 20 minutes.

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