• Title/Summary/Keyword: Rietveld method.

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Properties of Hexaferrite Co2Y(Ba2Co2Fe12O22) Prepared by Coprecipitation Method (공침법에 의해 제조된 육방정 산화철 Co2Y(Ba2Co2Fe12O22)의 특성)

  • 신형섭;이상걸;권순주
    • Journal of the Korean Ceramic Society
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    • v.29 no.3
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    • pp.195-201
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    • 1992
  • It had been studied the structure and the magnetic properties of singel phase Co2Y(Ba2Co2Fe12O22) powder, one of the hexagonal ferrite. The material was successfully prepared by a commercially applicable coprecipitation method. Adding asqueous solution of BaCl2, CoCl2 and FeCl2(Ba2+:Co2+:Fe2+=1:1:6 in mole ratio) to a mixture of NaOH and hydrogen peroxide solution, coprecipitate was formed with rapid oxidation of ferrous to ferric ion. The coprecipitate transformed to single phase Co2Y powder at heat treatment temperatures as low as 900$^{\circ}C$. The shape of Co2Y particles obtained at 900$^{\circ}C$ was hexagonal plate-like (diameter∼$\mu\textrm{m}$, aspect ratio>10). The structure of the Co2Y was refined by a Rietveld analysis of the measured X-ray diffractogram. The lattice parameters are ao=5.8602${\AA}$ and co=43.512${\AA}$. Co2Y is a soft magnetic material with saturation magnetization 30 emu/g and coecivity 170 . A standard X-ray diffraction pattern for Co2Y is proposed as well.

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Magnetic Properties of Sn1-xFexO2 Thin Films and Powders Grown by Chemical Solution Method

  • Li, Yong-Hui;Shim, In-Bo;Kim, Chul-Sung
    • Journal of Magnetics
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    • v.14 no.4
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    • pp.161-164
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    • 2009
  • Iron-doped $Sn_{1-x}Fe_xO_2$ (x = 0.0, 0.05, 0.1, 0.2, 0.33) thin films on Si(100) substrates and powders were prepared by a chemical solution process. The x-ray diffraction (XRD) patterns of the $Sn_{1-x}Fe_xO_2$ thin films and powders showed a polycrystalline rutile tetragonal structure. Thermo gravimetric (TG) - differential thermal analysis (DTA) showed the final weight loss above $430{^{\circ}C}$ for all powder samples. According to XRD Rietveld refinement of the powders, the lattice parameters and unit cell volume decreased with increasing Fe content. The magnetic properties were characterized using a vibrating sample magnetometer (VSM) and M$\ddot{o}$ssbauer spectroscopy. The thin film samples with x = 0.1 and 0.2 showed paramagnetic properties but thin films with x = 0.33 exhibited ferromagnetic properties at room temperature. Mossbauer studies revealed the $Fe^{3+}$ valence state in the samples. The ferromagnetism in the samples can be interpreted in terms of the direct ferromagnetic coupling of ferric ions via an electron trapped in a bridging oxygen deficiency, which can be explained using the F-center exchange model.

Effects of $Mn_2O_3, Y_2O_3$ Additives and Valence State of Mn ion in $Sr(Zr, Ti)O_3$ Microwave Dielectrics ($Sr(Zr, Ti)O_3$ 마이크로파 유전체에 첨가된 $Mn_2O_3, Y_2O_3$ 의 영향과 Mn의 산화상태)

  • 정하균;박도순;박윤창
    • Journal of the Korean Ceramic Society
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    • v.34 no.6
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    • pp.583-590
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    • 1997
  • The effects of Mn2O3 and Y2O3 additives on the microstructure and dielectric properties of Sr(Zr, Ti)O3 have been investigated. Powders with Sr(Zr1-xTix)O3(0$\leq$x$\leq$0.1) composition were prepared by the conventional solid state processing from commercial TiO2 and precipitation-processed ZrO2. The powders containing sintering additives of Mn2O3 and Y2O3 were compacted and then sintered at 1,55$0^{\circ}C$ for 4 h to get>97% relative density. Mn2O3 suppressed the grain growth and Y2O3 enhanced the density of sintered body. The oxidation state of Mn ions were determined by a chemical wet method and EPR spectroscopy. Mn ions were present as Mn2+ and Mn4+ in SrZrO3, while as Mn3+ and Mn4+ in Ti-substituted Sr(Zr, Ti)O3. With the substitution of Ti, the lattice parameters of SrZrO3 decreased and its dielectric constant increased with remarkable decrease in Q value. The dielectric constant of Sr(Zr, Ti)O3 was in the range of 30 to 40, Q values 1,200~5,400 at 6 GHz and temperature coefficient of resonant frequency -67~100 ppm/K.

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Synthesis of Aluminophosphate using Structure Directing Agent containing Piperidine Moiety: Effect of SDA on Crystal Structure (피페리딘 구조유도분자를 이용한 알루미노포스페이트 제올라이트 합성: 피페리딘 구조유도분자가 결정구조 형성에 미치는 영향)

  • Shin, Hye Sun;Jang, Ik Jun;Shin, Na Ra;Ju, Bit Na;Cho, Sung June
    • Korean Chemical Engineering Research
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    • v.49 no.5
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    • pp.657-663
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    • 2011
  • Structure directing agent(SDA) containing piperidine moiety such as piperidine(PI), 2-methylpiperidine (MPI), 2,6-dimethylpiperidine(DMPI) and 2,2,6,6,-tetramethylpiperidine(TMPI), respectively has been utilized to synthesize aluminophosphate zeolite using hydrothermal method. The gel composition was $1.0Al_2O_3:1.0P_2O_5:0.76SDA:45H_2O$ and the hydrothermal heating was performed in an oven at 443 K and for 7 days at static mode. The obtained zeolitic material contained a lamellar structure when PI was used as the SDA. With a progressive increase of the SDA size, various structures of aluminophosphate including AlPO-5 of AFI structure were obtained. The aluminophosphate of SAS structure was formed when the largest TMPI was utilized as the SDA, which was confirmed by the Rietveld refinement. The result of $^{27}Al$ and $^{31}P$ MAS NMR of the sample suggested that Al and P were incorporated into the framework of the aluminophosphate.

Phase transition and crystal structure analysis of PTCR $BaTiO_3$ ceramics with dopants (Y, Nb) (첨가제(Y, Nb)에 따른 PTCR $BaTiO_3$계 세라믹스의 결정구조 해석과 상전이 특성)

  • 차용원;원승신;백종후;이희수;엄우식;송준광;이인식;정훈택
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.2
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    • pp.253-258
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    • 1997
  • The characteristics of crystal structure and phase transition with dopants ($Nb_2O_5$= 0.1~0.4 mol% and $Y_2O_3$ : 0.2~0.4 mol%) on the PTCR $BaTiO_3$ system were investigated. In the case of $Nb_2O_5$ additive, the lattice parameter of PTCR $BaTiO_3$ was changed linearly with the increasement of $Nb_2O_5$ which substituted B-site of BaTiO$_3$ and the lattice parameter of c-axis decreased abruptly at 0.3 mol%. These phenonmena were assumed to originate from the distortion of octahedron and we could confirm that the change of lattice parameter accorded with the characteristics of the phase transition temperature. $Y^{3+}$ ions substituted both of A- and B-site until the 0.3 mol% addition, but $Y^{3+}$ substitution preferred A- to B-site above 0.3 mol%. This was affirmed by the variation ,of lattice parameter and the characteristics of phase transition. It also was found that $Y^{3+}$ions in the A-site substituted both of $Ba^{2+}$ and $Ca^{2+}$ ions with equal ratio by Rietveld method.

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Studies on Crystallographic and Magnetic Properties of the Sn0.9957Fe0.01O2 (Sn0.9957Fe0.01O2의 결정학적 및 자기적 성질에 관한 연구)

  • Li, Yong-Hui;Kim, Sam-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.20 no.5
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    • pp.187-190
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    • 2010
  • $Sn_{0.99}{^{57}Fe}_{0.01}O_2$ prepared by a sol-gel method, and studied by x-ray diffractometer, vibrating magnetometer, Superconducting quantum interference devices and M$\ddot{o}$ssbauer spectroscopy. the crystal structure were found to be a rutile tetragonal structure with space group $P4_2$/mnm, and oxygen deficiency are 5.6 % by Rietveld refinement. magnetization value were $M_s=1.95{\times}10^{-2}{\mu}_B/Fe$ at room temperature, and Curri-weiss temperature were and ${\theta}_{cw}$ = 18 k, measurement of VSM and SQUID, respectively. Mssbauer spectra of $Sn_{0.99}{^{57}Fe}_{0.01}O_2$ have been Sextet taken at various temperatures ranging from 4.2 K to RT, and isomer shift value $\delta$ = 0.18~0.36 mm/s of $^{57}Fe$ ion site all of the temperature range the state shows ferric.

Analysis of the Crystal Structure and the Relation with the Temperature Coefficient au_\varepsilon$ in $BaORe_2O_3TiO_2$ (Re=La, Nd, Y) Microwave Dielectric Ceramics ($BaORe_2O_3TiO_2$ (Re=La, Nd, Y)계 고주파 유전체의 결정구조 분석 및 온도계수 au_\varepsilon$와의 관련성)

  • 김정석;강현주;심해섭;이창희;천채일
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.136-144
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    • 1999
  • Crystal structures of tungsten-bronze type microwave dielectric ceramics, $BaOLa_2O_34TiO_2$ (BLT) and $BaO(Nd_{0.77}Y_{0.23})_4TiO_2$ (B(NY)T), were analysed using the Rietveld method. The most relibale refinement was obtained by refining the cation and anion positions from the x-ray and neutron diffraction data, respectively. The ambiguites inherent in the refined crystal structure by Mateeva et al. were resolved. The $BaORe_2O_34TiO_2$ structure consiste of $3\times2$ perovskite blocks and 4 pentagon-channels. The Ti-O6 octahedrons are distroted and tilted, which, consequently, induces the displacements of Ba and Re ions producing the superlattics (c$\approx$ 7.6 $\AA$). The B(NY)T showed more severely tilted Ti-O6 octahedrons. The relative dielectric constant $\varepsilon_{\gamma}$ and temperature coefficient $\tau_\varepsilon$ are 109.5 and-$180 ppm/^{\circ}C$ in BLT, 76 and $+40 ppm/^{\circ}C$ in B(NY)T, respectively. The small Re ions produced a positive $\tau_\varepsilon$. The relation between $\tau_\varepsilon$ and the octahedron tilting in complex perovskite is discussed for the tungsten bronze type structure.

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Evaluation of Hydration Characteristics and NOx-removal Performances of Cement Paste Containing Refined TiO2 Obtained from Waste Sludge (폐수 슬러지에서 정제된 TiO2를 혼입한 시멘트 페이스트의 수화특성 및 질소산화물 제거 성능 평가)

  • Yoon, Hyunno;Seo, Joonho;Kim, Seonhyeok;Bae, Jinho;Kil, Taegeon;Lee, Haeng-Ki
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.41 no.4
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    • pp.357-364
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    • 2021
  • The present study investigated the hydration properties and NOx-removal performances of the cement pastes containing three different types of TiO2. Two commercially available TiO2 (P-25 and NP-400) and refined TiO2 (GST) obtained from waste sludge were incorporated to cement paste at levels of 0, 5, 10, and 20 wt%. Isothermal calorimetry test results indicated that the TiO2 incorporation induced a notable influence on the reaction kinetics of cement paste, showing the highest cumulative heat release in the samples containing P-25, followed by NP-400 and GST. Quantitative X-ray diffractometry as calculated by the Rietveld method identified that the incorporated TiO2 promoted the formation of C-S-H, ultimately leading to the enhancement in the 28 day-compressive strength of cement pastes. As revealed by SEM/EDS analysis, the content of distributed Ti elements on the surface of the samples was in the order of P-25, GST, and NP-400. Regardless, the NOx-removal performance was the highest in the sample containing P-25, followed by NP-400 and GST.

Dielectric Properties of (Ba0.7Sr0.3-3x/2Lax)(Ti0.9Zr0.1)O3 Ceramics with La3+ Substitution for Sr2+-Site ((Ba0.7Sr0.3-3x/2Lax)(Ti0.9Zr0.1)O3 세라믹의 Sr2+-자리에 대한 La3+ 치환에 따른 유전 특성)

  • Si Hyun Kim;Ju Hye Kim;Eung Soo Kim
    • Korean Journal of Materials Research
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    • v.33 no.11
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    • pp.465-474
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    • 2023
  • The effects of La3+ substitution for Sr2+-site on the crystal structure and the dielectric properties of (Ba0.7Sr0.3-3x/2Lax) (Ti0.9Zr0.1)O3 (BSLTZ) (0.005 ≤ x ≤ 0.02) ceramics were investigated. The structural characteristics of the BSLTZ ceramics were quantitatively evaluated using the Rietveld refinement method from X-ray diffraction (XRD) data. For the specimens sintered at 1,550 ℃ for 6 h, a single phase with a perovskite structure and homogeneous microstructure were observed for the entire range of compositions. With increasing La3+ substitution (x), the unit cell volume decreased because the ionic size of La3+ (1.36 Å) ions is smaller than that of Sr2+ (1.44 Å) ions. With increasing La3+ substitution (x), the tetragonal phase fraction increased due to the A-site cation size mismatch effect. Dielectric constant (εr) increased with the La3+ substitution (x) due to the increase in tetragonality (c/a) and the average B-site bond valence of the ABO3 perovskite. The BSLTZ ceramics showed a higher dielectric loss due to the smaller grain size than that of (Ba0.7Sr0.3)(Ti0.9Zr0.1)O3 ceramics. BSLTZ (x = 0.02) ceramics met the X7R specification proposed by the Electronic Industries Association (EIA).

Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.853-856
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    • 2006
  • Dion-Jacobson phases $CsCa_2Nb_2FeO_9$ and $CsCa_2Nb_2AlO_9$ were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of $NbO_6-MO_4-NbO_6$ in tripled slab, in fact, were mixed phases of n = 3 Dion-Jacobson phases and impurities such as $Ca_2NbFeO_6$ and $Ca_3Al_2O_6$. The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of $CsCa_2Nb_2FeO_9$ was calculated into $Cs_{0.59}Ca_{2.64}Nb_{2.92}Fe_{0.81}$ in small agglomerate crystals and $Cs_{0.95}Ca_{1.97}Nb_{3.08}Fe_{0.15}$ in long plate-like crystals.