• Title/Summary/Keyword: XRD분석

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Effect of Annealing on Structural and Electrical Properties of VOx Thin Films (VOx 박막의 구조적 특성과 전기적 특성에 대한 열처리 영향)

  • Lee, Jang Woo;Chung, Chee Won
    • Applied Chemistry for Engineering
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    • v.17 no.5
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    • pp.471-475
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    • 2006
  • $VO_x$ thin films with the thickness of 450 nm were prepared on a $Pt/Ti/SiO_{2}/Si$ substrate at room temperature by a reactive radio frequency (rf) magnetron sputtering method. The deposition rates of $VO_x$ thin films were investigated as a function of $O_{2}$ concentration and rf power. As the $O_{2}$ concentration in a $O_{2}/Ar$ mixture increased, the deposition rate decreased. However, the deposition rate increased with increasing rf power. The deposited $VO_x$ thin films were annealed at $450^{\circ}C$ for 2, 4, and 6 h in $O_{2}$ and $N_{2}$ ambient. After annealing, the phase changes of $VO_x$ thin films were investigated using X-ray diffraction analysis. The plane and cross-sectional views of $VO_x$ thin films before and after annealing were observed by field emission scanning electron microscopy. The metal-insulator transition (MIT) properties of $VO_x$ thin films were measured using current-voltage measurement. The excellent MIT properties were observed in $VO_x$ thin films annealed in $O_{2}$ ambient.

Study of a Supercritical Fluid Process for the Preparation of Hydroxypropyl-β-cyclodextrin Inclusion Complexes (Hydroxypropyl-β-cyclodextrin 포접복합체 제조를 위한 초임계유체 공정 연구)

  • Lee, Sang-Yun;Kim, Jeong-Kyu;Kim, Woo-Sik;Ryu, Jong-Hoon;Lim, Gio-Bin
    • Korean Chemical Engineering Research
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    • v.43 no.1
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    • pp.110-117
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    • 2005
  • In this work, solid-state inclusion complex powders of itraconazole and $2-hydroxypropyl-{\beta}-cyclodextrin(HP-{\beta}-CD)$ were produced by a supercritical anti-solvent (SAS) process. In order to evaluate the degree of complexation, the thermal behavior of the microparticulate complexes was investigated using differential scanning calorimetry. The experimental results obtained for the solubility and dissolution rate of the microparticulate inclusion complexes in a buffer solution of pH 1.2 showed that the complexation of itraconazole with $HP-{\beta}-CD$ results in a significant increase in the solubility and dissolution rate of itraconazole. The particle size of the SAS-produced inclusion complexes was dramatically reduced ($<0.1-0.5{\mu}m$) compared with untreated itraconazole ($30-50{\mu}m$) and $HP-{\beta}-CD$ ($50-100{\mu}m$). The solubility of itraconazole was increased with the increase of pressure at a constant temperature to ca. $758.6{\mu}g/mL$ in an aqueous medium of pH 1.2. The dissolution rate of itraconazole was observed to be significantly improved and about 90% of itraconazole was found to be dissolved within 5-10 min.

The Solidification Characteristics of Recycled Aggregate Mixed with Incineration Ash and Waste Concrete (소각재와 폐콘크리트를 이용한 재생골재의 고형화 특성)

  • Yeon, Ikjun;Ju, Soyoung;Lee, Sangwoo;Shin, Taeksoo;Kim, Kwangyul
    • Journal of the Korean GEO-environmental Society
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    • v.9 no.5
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    • pp.5-13
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    • 2008
  • In this study, It was carried out to evaluate the feasibility of recycled crushed concrete as aggregate used cement mortar replace sand and to investigate engineering properties of recycled aggregate for hazardous waste solidification. The compressive strength of cement mortar replaced 5-15% (wt.) recycled aggregate was over $163kgf/cm^2$ which is the standard of first grade concrete block class C. And cement mortar was examined to evaluate the stability by leaching test. Cu, Cd, Pb, Cr, and As as the heavy metals were proved very stable but mercury (Hg) was leached high concentration because it was simply tied to the cement surface. We investigated the crystal structures of cement mortar and they had shown the peaks of $Ca(OH)_2$, ettringite, and CSH (calcium silicate hydrate). As the result, the longer curing time, the higher CSH peak that means to increase compressive strength and the cement mortar was more stable. Therefore it was shown that it may be possible to apply hazardous waste solidification using recycled aggregate, fly ash and sewage sludge ash.

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Electrochemical Properties of Spinel LiMn2O4 Prepared Through Different Synthesis Routes (스피넬형 양극활물질 LiMn2O4의 합성방법에 따른 전기화학적 특성 비교)

  • Lee, Ki-Soo;Bang, Hyun-Joo;Sun, Yang-Kook
    • Journal of the Korean Electrochemical Society
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    • v.10 no.1
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    • pp.48-51
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    • 2007
  • In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.

Superconductivity of High $T_c$ Superconductor $(Y_{1-x}Eu_x)Ba_2Cu_3O_{7-{\delta}}$ (고온초전도체 $(Y_{1-x}Eu_x)Ba_2Cu_3O_{7-{\delta}}$의 초전도성)

  • Chung Won Yang;Kweon Jung Ohk;Cho Eun Kyung;Kim Keyung Nam;Han, Sang Mok
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.16-23
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    • 1992
  • High $T_c$, superconductor $(Y_{1-x}Eu_x)Ba_2Cu_3O_{7-{\delta}}$ (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared and the physical properties were observed. XRD analysis showed that the structures of all the specimen were orthorhombic and the lattice parameters a, b and c increased with the increasing x value. Electrical resistivity and magnetization measurements revealed that pure high $T_c$, superconducting phases were formed at above 90 K. The critical temperatures increased with increasing the amount of Eu. From the measurement of magnetization and the size of the grains using SEM micrographs, volume diamagnetic susceptibilities for each specimen were calculated. These values decreased with the increasing x value. The composition of Ba in the lattice site decreased as the concentration of Eu increased, and this was confirmed by EPMA. It was found out that the volume diamagnetic susceptibility of each specimen was directly influenced by the composition of Ba in the lattice site.

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The optical and structural properties by ZrO2 and Y2O3 compositional ratio of Co- and Ce-doped cubic zirconia (YSZ) single crystals (ZrO2와 Y2O3 조성비에 따른 Co와 Ce 첨가 큐빅지르코니아(YSZ) 단결정의 광학적 및 구조적 특성)

  • Moon, So-I.;Park, Hee-Yul;Seok, Jeong-Won
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.2
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    • pp.73-77
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    • 2012
  • Co-(0.8 wt%) and Ce-(0.4 wt%) doped cubic zirconia ($ZrO_2$ : $Y_2O_3$ = 80 : 20, 70 : 30, 60 : 40, 50 : 50 wt%) single crystals grown by a skull melting method were heat-treated in $N_2$ at $1000^{\circ}C$ for 5 hrs. The orange, yellowish brown and brown colored as-grown single crystals were changed into either brownish red, yellow and green color after the heat treatment. Before and after the heat treatment, the YSZ (yttria-stabilized zirconia) single crystals were cut for wafer form (${\phi}6.5mm{\times}t2mm$). The optical and structural properties were examined by UV-VIS spectrophotometer and X-ray diffraction. Absorption by $Ce^{3+}(^2F_{5/2,7/2}(4f){\rightarrow}^2T_g(5d^1))$, $Co^{2+}(^4A_2(^4F){\rightarrow}^4T_1(^4F)$ or $^4T_1(^4P))$ and $Co^{3+}$, change of ionization energy and lattice parameter were confirmed.

Effect of modifiers on the properties of glass-ceramics containing coal bottom ash (석탄 바닥재가 포함된 결정화 유리의 특성에 미치는 수식제의 영향)

  • Kang, Seung-Gu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.1
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    • pp.53-57
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    • 2010
  • The influence of CaO addition on the crystallization temperature, crystal types, and microstructure of L-A-S ($Li_2O-Al_2O_3-SiO_2$) glass-ceramics system fabricated from a coal bottom ash, produced at thermal power plant, was studied. The glass transition and crystallization temperatures were shifted to the higher temperature position with increasing CaO content in a non-isothermal analysis using a DTA. The major crystalline phases of L-A-S glass-ceramics system produced were identified as ${\beta}$-spodumene ($LiAlSi_2O_6$) and eucryptite ($LiAlSiO_4$). The glass-ceramics showed a bulk and surface crystallization behavior at a time. With increasing CaO content, the ${\beta}$-spodumene peak in XRD increased and some CaO-related phases were formed. The surface crystal grown from the exterior to the center in glass-ceramics showed various shapes by amount of CaO added. Some cracks were generated at the glass-ceramics containing CaO above 9 wt% due to the mismatch of thermal expansion coefficients between a ${\beta}$-spodumene and CaO-related crystal phases.

Synthesis and Characterization of Epoxy Silane-modified Silica/Polyurethane-urea Nanocomposite Films (에폭시 변성 실리카 나노입자/폴리우레탄-우레아 나노복합체 필름의 제조 및 특성 연구)

  • Joo, Jin;Kim, Hyeon Seok;Kim, Jin Tae;Yoo, Hye Jin;Lee, Jae Ryung;Cheong, In Woo
    • Korean Chemical Engineering Research
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    • v.50 no.2
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    • pp.371-378
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    • 2012
  • Hydrophilic silica nanoparticles (SNPs) were treated by using 3-glycidoxypropyltrimethoxy silane (GPTMS) and then they were blended with polyurethane-urea (PUU) emulsions to obtain SNPs/PUU nanocomposite films. Thermo-mechanical properties of the nanocomposite films were investigated by varying the grafted amount of GPTMS onto SNPs and the contents of SNPs in the PUU matrix. The thermo-mechanical properties of the nanocomposite films were also compared in terms of the dispersibility of SNPs in the PUU matrix and thermal curing of the GPTMS-grafted SNPs. The maximum amount of grafted GPTMS was $1.99{\times}10^{-6}\;mol/m^2$, and which covered ca. 53% of the total SNP surface area. $^{29}Si$ CP/MAS NMR analyses with the deconvolution of peaks revealed the details of polycondensation degree and patterns of GPTMS in the surface modification of SNPs. The surface modification did not significantly affect colloidal stability of the SNPs in aqueous medium; however, the hydrophobic modification of SNPs offered a favorable effect on the dispersibility of SNPs in the PUU matrix as well as better thermal stability. XRD patterns revealed that GPTMS-grafted SNPs broadened the reduced the characteristic peak of polyol in PUU matrix. The composite films became rigid and less flexible as the SNP content increased from 5 wt.% to 20 wt.%. Particularly, Young's modulus and tensile modulus significantly increased after the thermal curing reaction of the epoxy groups in the SNPs.

Exchange-coupling Interaction and Magnetic Properties of BaFe12O19/Ni0.5Zn0.5Fe2O4 Nanocomposite Ferrite (BaFe12O19/Ni0.5Zn0.5Fe2O4 나노복합체 Ferrite의 Exchange-coupling 상호 작용과 자기 특성)

  • Oh, Young-Woo
    • Journal of the Korean Magnetics Society
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    • v.24 no.3
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    • pp.81-85
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    • 2014
  • Nano-sized Ba-ferrite, Ni-Zn ferrite and $BaFe_{12}O_{19}/Ni_{0.5}Zn_{0.5}Fe_2O_4$ nanocomposite ferrite were prepared by sol-gel combustion method. Nanocomposite was calcined at temperature range of $600{\sim}900^{\circ}C$ for 1 h. According to the diffraction patterns, hard/soft nanocomposite was indicated to the coexistence of the magnetoplumbite structural $BaFe_{12}O_{19}$ and spinel $Ni_{0.5}Zn_{0.5}Fe_2O_4$ and agree with the standard data (JCPDS 10-0325). The particle size of nanocomposite turn out to be less than 90 nm. The nanocomposite ferrite shows a single-phase magnetization behavior, implying that the hard magnetic phase and soft magnetic phase were well exchange-coupled. The specific saturation magnetization ($M_s$) of the nanocomposite is located between hard ($BaFe_{12}O_{19}$) and soft ferrite ($Ni_{0.5}Zn_{0.5}Fe_2O_4$). The remanence (Mr) of nanocomposite ferrite is much higher than that for the individual $BaFe_{12}O_{19}$ and $Ni_{0.5}Zn_{0.5}Fe_2O_4$ ferrite. $(BH)_{max}$ is increased, generally.

C2H5OH-CH2OHCH2OH-Ca(OH)2-CO2계에서의 비정질탄산칼슘의 결정화 연구

  • Kim, Hwan;Ahn, Ji-Whan
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.3-27
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    • 1996
  • 분체의 입자 배열이 불규칙한 경우뿐만 아니라 입자 크기가 극미세하여 X선회절분석이 불가능한 경우에도 비정질물질이라 한다. 수용액 속에서 이런 비정질 물질을 합성하기 위해서는 합성용액의 과포화도를 높여 계속 유지시킴에 따라 극미세 1차핵 생성의 지속적인 유도에 따른 입자 성장을 최대한 억제시켜야만 한다. 본 연구에서는 흡습제, 칼슘제 및 식품 첨가제 등으로 이용되는 비정질 탄산칼슘을 계에서 합성하고, 이때 생성된 비정질 상태의 겔을 수용액 환경을 변화시켜가면서 따라 결정화를 유도하고 탄산칼슘의 동질이상을 관찰하였다. CO2의 유속을 11/min, 교반속도를 600rpm으로 고정시키고, Ca(OH)2의 양을 10g에서 50g까지 변화시켜가면서 겔 상태의 비정질 탄산칼슘을 합성하였다. 이때 전기전도도는 CO2의 용해와 더불어 Ca(OH)2의 용해도가 증가함에 따라 변화하였으며, 반응종반부에는 겔화가 시작될 때까지 거의 일정하였다. 따라서, 이러한 사실들로부터 현탁액 내에서의 전기전도도의 변화는 Ca이온의 영향을 받는 것으로 사료된다. 비정질 탄산칼슘은 수용액에서 불안정하여 CO2 가스를 방출하면서 급격히 결정화되는데, 본 연구에서는 Ca(OH)2의 양을 20g으로 하여 위의 방법에 의해 얻어진 겔을 수용액의 종류와 농도 및 결정화 온도, 교반속도를 달리하면서 결정화시켰다. 교반속도를 100rpm으로 하여 물의 온도변화에 다라 결정화시킨 경우 전 온도범위에서 칼사이트상이었으며, 물의 온도가 5$^{\circ}C$일 경우에는 미세한 입자들이 응집된 형태였으나, 그 외의 온도변화조건에서는 모두 평균입경 0.4$\mu\textrm{m}$정도의 비교적 균일하 능면체 형태였다. 또한 교반속도를 500rpm으로 증가시켰을 경우에는 8$0^{\circ}C$에서 침상의 아라코나이트가 소량생성되었음을 SEM사진으로 관찰할 수 있었으며, 소량의 바테라이트도 혼재되어 결정화되었음을 XRD결과로 알 수 있었다. 교반속도를 100rpm으로 한 NH4Cl 0.5mol/l 수용액에서는 입자의 형태와 크기가 불규칙한 칼사이트로 결정화되었으며, MgCl2 0.05mol/l 수용액의 경우에는 순수한 H2O의 경우에서와는 달리 2$0^{\circ}C$에서는 모서리가 무딘 매우 균일한 크기의 칼사이트 입자가 관찰되었으며, 6$0^{\circ}C$부터는 아라고나이트가 생성됨을 관찰할 수 있었다. 따라서, 고온(8$0^{\circ}C$)의 농도 MgCl2 수용액(0.1, 0.2 mol/l)에서 교반속도를 높여(800rpm) 겔을 결정화시킨 결과 아라고나이트의 생성수율이 증가되는 것을 확인할 수 있었다.

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