• Title/Summary/Keyword: X-선 분말회절

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Modified Sol-Gel Processing for Titanium Disulfide (졸겔법을 응용한 이황화티탄늄의 합성에 관한 연구)

  • Go, Yong Bok;Bae, Young Je;Chae, Hee K.
    • Journal of the Korean Chemical Society
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    • v.41 no.3
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    • pp.130-137
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    • 1997
  • Powders and thin-layers of a hexagonal titanium disulfide phase have been successfully prepared by modifying the sol-gel process. The reaction of titanium isopropoxide with hydrogen sulfide causes the precipitation of a precursor which was converted to the disulfide on heat-treatment in $H_2S$ at various temperatures depending on the solvent adopted, whereas that of titanium 2-methoxyethoxide with $H_2S$ produces a stable solution which was spin-casted onto silicon substrates followed by thermolysis to give thin films. Upon heat-treatment in $H_2S$, the disulfides show interesting morphological variations in the form of their powders and thin films, which were characterized by SEM and X-ray diffractometer.

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Preparation of $Pb(Sc_{1/2}Ta_{1/2})O_3$, by the molten salt synthesis method (용융염 합성법에 의한 $Pb(Sc_{1/2}Ta_{1/2})O_3$의 제조)

  • Park, Kyung-Bong;Kim, Tae-Huei
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.15 no.3
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    • pp.99-103
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    • 2005
  • Lead scandium tantalate powders were prepared by a molten salt synthesis method using NaCl-KCl as a flux. Variations in phase formation and particle morphology were investigated for the temperature range from $700^{\circ}C\;to\;800^{\circ}C$. $Pb(Sc_{1/2}Ta_{1/2})O_3$, with pure perovskite phase was formed at $750^{\circ}C$ fur 2 hrs and the prepared powder had the cubic-like morphology and the average particle size below $0.5{\mu}m$. The results were discussed with respect to DTA, X-ray diffraction, and microstructural characterization data.

An Study on the Structure of Maghemite(${\gamma}$-Fe$_2$O$_3$) I -Rietveld Analysis of Powder XRD Patterns- (마게마이트(${\gamma}$-Fe$_2$O$_3$)대한 연구 I -분말 X-선 회절무늬의 Rietveld 분석-)

  • 신형섭
    • Journal of the Korean Ceramic Society
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    • v.35 no.10
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    • pp.1113-1119
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    • 1998
  • Crystal structure of needle-shaped maghemite(${\gamma}$-{{{{ { {Fe }_{2 }O }_{3 } }}) has been studied by the Rieveld analysis of powder X-ray diffraction patterns. The tetragonal space group P41,.3212 and cubic space group P41,.32 have been have been used for the refinement of X-ray diffraction patterns. The crystal system of maghemite is closed to tetragonal more than cubic. The tetragonal lattice parameters are a=8.3460$\AA$ and c=25.034$\AA$ The standard X-ray diffraction pattern of the tetragonal maghemite analyzed with space group P41,.3212 is proposed.

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Structural and Photoluminescence Properties of Sr1-1.5xMoO4:Eux3+ Phosphors

  • Ryu, Geun-Taek;Jo, Sin-Ho
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2012.05a
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    • pp.195-195
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    • 2012
  • $Eu^{3+}$ 이온의 농도비를 변화시키면서 고상 반응법을 사용하여 적색 형광체 $Sr_{1-1.5x}MoO_4:Eu_x{^{3+}}$ 분말을 합성하였다. 제조한 형광체의 결정 구조는 X-선 회절 장치를 사용하여 정방정계임을 확인하였고, 광학 특성은 형광 광도계를 사용하여 상온에서 측정하였다. $Eu^{3+}$ 이온의 농도비가 0.01 mol인 형광체의 경우에, 파장 295 nm로 여기시켰을 때 주된 발광은 파장 619 nm에 최대 세기를 갖는 적색 형광을 나타내었으며, 최대 흡수 스펙트럼은 넓은 밴드를 갖고 파장 302 nm에서 관측되었다.

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Comparative Crystal Chemistry of Exchanged by Cs-, Cd-, Pb-, and Sr-synthetic Mordenite Using High Resolution X-ray Powder Diffraction (고분해능 X-선 분말 회절을 이용한 Cs-, Cd-, Pb-, Sr-으로 치환된 합성 모데나이트의 격자상수 비교 연구)

  • Lee, Soojin;Lee, Hyunseung;Seoung, Donghoon;Kim, Pyosang;Kim, Hyeonsu;Lee, Yongmoon
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.3
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    • pp.345-353
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    • 2022
  • This study aimed to fundamentally understand changes of cell parameters of cation-exchanged mordenites using high resolution X-ray powder diffraction for studies that immobilization of various heavy metal cation using synthesis mordenite (Na6.6Al6.6Si41.4O96·20.4H2O, Na-MOR). As a results of measurement by Thermogravimetric analysis (TGA), it was confirmed that 19.4, 20.4 water molecules per unit cell were present in monovalent-cation substituted MOR (Cs-MOR, Na-MOR), and 21, 23.1, 23.2 water molecules per unit cell were present in divalent-cation substituted MOR (Pb-MOR, Sr-MOR, Cd-MOR). The space group of all the samples were identified as Cmcm belonging to the orthorhombic crystal system. Compared to Na-MOR, starting material, relative peak intensity of (110) and (200) is significantly changed after cation substitution whereas peak position is almost similar. Also, (220) peak that was not found in Na-MOR was clearly observed in Pb-, Cd- and Sr-exchanged MOR. Thus, it was estimated that changes of atomic distribution usually occurred on ab-plane while changes of cell parameters were little. Detailed changes in the cell parameters of cation-exchanged mordenites were derived from whole profile fitting method using the GSAS suite program. Changes in the axial lengths and unit cell volume of cation substitution showed different relationship depending on ionic radius and charge number. In case of monovalent-cation substituted MOR, the length of a-axis increases whereas the length of b- and c-axis decrease by absorbed cation radius. In the case of divalent-cation exchanged MOR, the length of a-axis usually decreases while the length of b- and c-axis increases by cation radius. It was confirmed that unit cell volume of monovalent and divalent cation substituted MORs had an independent tendency by cation radius.

Characterization and preparation titanate nanotubes for Li-ion secondary battery (Li 이차전지용 티타네이트 나노튜브 제조 및 특성평가)

  • Oh, Hyo-Jin;Lee, Nam-Hee;Yoon, Cho-Rong;Jung, Sang-Chul;Kim, Sun-Jae
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.510-510
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    • 2007
  • Titanate nanotube(TNT)는 높은 비표면적과 우수한 물리화학적 특성을 가지고 있어 광촉매, 수소 저장재료, 태양전지용 전극재료 등에 적용되고 있다. 또한, 티타네이트 나노튜브는 전자 이동이 원활한 구조적 특징을 가지고 있어 리듐 이차전지용 호스트 재료로서 많은 연구가 진행 중이다. 이에 본 연구에서는 저온균일침전법으로 제조한 루틸상 $TiO_2$ 분말에 Lithium chloride를 1~10wt%를 동시에 첨가한 후 10M의 sodium hydroxide 수용액 내에서 수열합성하여 리튬이 도핑된 티타네이트 나노튜브를 제조하였다. 제조된 분말의 입자형상 및 크기는 전자주사 현미경을 이용하여 관찰하였으며, X-선 회절분석을 이용하여 리튬 첨가에 따른 결정상 변화를 관찰하였다. 또한 리튬이 도핑된 티타네이트 나노튜브의 전기화학적 특성 평가를 위해 양극 활물질 : 도전제 : 바인더를 75 : 20 : 5의 비율로 혼합한 후 coin cell을 제조하였고, potentiostat를 이용하여 용량 측정 및 cycle 특성을 실시하였다. 수열 합성법에 의해 형성된 입자는 직경 10nm, 길이 수 ${\mu}m$로 관찰되었으며, X-선 회절 시험 결과 LiO와 같은 이차상은 발견되지 않았다. 측정된 coin cell의 용량은 240mAh/g을 나타내었으나, 싸이클 특성이 빠르게 저하됨을 확인할 수 있었다.

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Sintering of $\textrm{TiH}_2$ Powders ($\textrm{TiH}_2$ 분말의 소결)

  • Kim, Won-Baek;Choi, Good-Sun;Suh, Chang-Youl;Kil, Dae-Sup;Ha, Ho
    • Korean Journal of Materials Research
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    • v.9 no.3
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    • pp.282-289
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    • 1999
  • 티타늄 수소화물(TiH$_2$) 분말을 원료로 사용하여 Ti 소결체를 제조하였다. 원료분말은 수소화-탈수소화법(HDH법)에 의해 제조한 상용분말이었으며 비교를 위해 동일한 입도를 갖는 Ti 분말도 함께 소결하였다. $TiH_2$는 소결체의 밀도를 현저하게 촉진하였으며 $TiH_2$$\longrightarrow$$Ti+H_2$의 탈수소반응에 의해 생성되 청정한 Ti분말이 소결을 촉진하기 때문인 것으로 판단된다. 같은 이유로 $TiH_2$소결체의 산소농도는 Ti 소결체보다 낮게 나타났다. 소결체의 잔류수소는 소결온도가 증가함에 따라 감소하였으며 $1200^{\circ}C$ 이상에서는 5 ppm 이하의 낮은 값을 나타냈다. 소결체의 경도는 소결밀도 및 산소량에 비례하는 것으로 나타났다. $TiH_2$분말의 cubic$\longrightarrow$tetragonal 변태온도는 X-선 회절분석 결과 $16~20^{\circ}C$ 구간으로 밝혀졌다.

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Synthesis and Characterization of Some Transition Metal Complexes of Unsymmetrical Tetradentate Schiff Base Ligand (비대칭 Tetradentate Schiff 염기 리간드의 전이금속 착물에 대한 합성 및 특성)

  • Munde, A. S.;Jagdale, A. N.;Jadhav, S. M.;Chondhekar, T. K.
    • Journal of the Korean Chemical Society
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    • v.53 no.4
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    • pp.407-414
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    • 2009
  • The solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with 4-hydroxy-3-(1-{2-(2-hydroxybenzylidene)- amino phenylimino}-ethyl)-6-methy-pyran-2-one (H2L) derived from o-phenylenediamine, 3-acetyl- 6-methyl-(2H) pyran, 2,4 (3H)-dione (dehydroacetic acid or DHA) and salicylic aldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, IR, $^1H$-NMR spectra, X-ray diffraction, thermal analysis, and screened for antimicrobial activity. The IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests square planar geometry for Cu(II) and Ni(II) complexes and octahedral geometry for Co(II), Mn(II) and Fe(III) complexes. The x-ray differaction data suggests orthorhombic crystal system for Cu(II) complex, monoclinic crystal system for Ni(II), Co(II) and Fe(III) and tetragonal crystal system for Mn(II) complex. Thermal behaviour (TG/DTA) of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus Niger and Trichoderma.

Sintering behavior of $\textrm{La}_{0.68}\textrm{Ca}_{0.32}\textrm{Cr}_{0.97}\textrm{O}_{3}$ Interconnector Material for SOFC (SOFC용 $\textrm{La}_{0.68}\textrm{Ca}_{0.32}\textrm{Cr}_{0.97}\textrm{O}_{3}$연결재료의 소결거동)

  • Lee, Yu-Gi;Park, Jong-Wan
    • Korean Journal of Materials Research
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    • v.7 no.4
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    • pp.276-286
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    • 1997
  • SOFC용 L $a_{0.68}$Ca/ sub 0.32/C $r_{0.97}$ $O_{3}$분말은 수산염법에 의해 제조되었고, 이 합성된 분말을 이용한 슬러리의 최적제조조건과 그린 필름의 최적 소성조건을 얻었으며,이 제조 조건에서 소결 시간과 온도에 따라 제조된 연결재료의 결정구조, 미세구조 및 소결거동을 각각X-선 회절, 주사전자현미경 그리고 에너지 분산 분광계를 이용하여 조사하였다. L $a_{0.68}$C $a_{0.32}$C $r_{0.97}$ $O_{3}$의 저온소결은 $Ca_{m}$ (Cr $O_{4}$)$_{n}$에 의해 이루어졌음이 관찰되었고, 이때 $Ca_{m}$ (Cr $O_{4}$)$_{n}$은 불규칙하게 녹아서 L $a_{1-x}$C $a_{x}$Cr $O_{3-}$$\delta$/와 반응하고 이 현상이 질량 이동을 증가시켜 시편의 급격한 결정립 성장과 조밀화를 야기시켰다. 이러한 결정립 성장과 조밀화는 소결온도 140$0^{\circ}C$부터 일어났다.X>부터 일어났다.

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Synthesis and characterization of $BaTiO_3$ fine particles by hydrothermal process (수열합성법에 의한 미립의 $BaTiO_3$ 분말합성 및 특성)

  • 배동식;주기태;한경섭;최상흘
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.4
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    • pp.563-566
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    • 1998
  • $BaTiO_3$ fine particles were prepared by hydrothermal process from titanium tetra-isoproproxide ($Ti(OiPr)_4$) and barium hexa-hydroxide ($Ba(OH)_2{cdot}8H_2O$) as raw materials. The fine particles were obtained at the temperature range of 160 to $185^{\circ}C$. The properties of $BaTiO_3$ particles were studied as a function of various parameters such as reaction temperature, reaction time and Ba/Ti ratio, etc. The average particle size of $BaTiO_3$ increased with increasing reaction temperature and time. After hydrothermal treatment at $170^{\circ}C$ for 8 h, the average particle size of $BaTiO_3$ was about 30 nm and the particle size distribution was narrow.

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