• 제목/요약/키워드: rietveld analysis

검색결과 84건 처리시간 0.029초

산화우라늄의 결정구조 분석 (Crystal Structure Analysis of Uranium Oxides)

  • 김정석;최용남;이창희;김시향;이영우
    • 한국세라믹학회지
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    • 제38권11호
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    • pp.967-972
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    • 2001
  • $UO_2$계 핵연료재료에서 O/U 비가 2.0, 2.03, 2.14, 2.19, 2.20 및 2.26인 시료들에 대한 중성자회절 데이터를 rietveld 정밀화를 이용하여 결함 및 결정구조, 온도에 따른(상온~100$0^{\circ}C$) 상변화 등을 분석하였고, 이를 상태도와 비교하였다. O/U 비가 2.14, 2.19, 2.20인 시료는 모두 $UO_{2+x}$$U_4$$O_{9}$ 두 상이 혼합된 것으로 분석되었고, 온도가 증가함에 따라 $UO_{2+x}$의 양이 증가하였다. $UO_{2+x}$는 공간군 Fm3m(a≒5.4$\AA$)으로, $U_4$$O_{9}$은 143d(a≒21.8$\AA$)로 분석되었다. $UO_{2.2}$$UO_{2.18}$에서 중성자회절 데이터를 이용한 온도에 따른 상분석 결과와 상태도로부터 예측되는 변화 경향은 대체로 일치하였으나, 부분적으로 차이를 나타내었다. 문헌에서 보고된 $U_4$$O_{9}$상의 ${\gamma}$$\longrightarrow$$\beta$$\longrightarrow$$\alpha$로의 상전이를 상분해와 연관하여 고찰하였다.고찰하였다.하였다.다.하였다.

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

  • 윤현노;서준호;김선혁;배진호;길태건;이행기
    • 대한토목학회논문집
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    • 제41권4호
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    • pp.357-364
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    • 2021
  • 본 연구에서는 서로 다른 종류의 TiO2 혼입이 시멘트 페이스트의 수화특성 및 질소산화물 제거성능에 미치는 영향에 대해 조사하였다. 상용 제품인 P-25와 NP-400, 폐수 슬러지에서 제조된 GST, 총 세 종류의 TiO2를 시멘트 무게대비 0, 5, 10, 20 % 첨가하여 시멘트 페이스트의 수화특성 및 질소산화물 제거성능을 분석하였다. 미소수화열 측정결과 TiO2의 혼입은 시멘트 페이스트의 초기 수화반응에 큰 영향을 미치는 것이 확인되었으며, P-25, NP-400, GST 순으로 더 높은 누적 발열량을 나타내었다. 이로 인해 Rietveld 분석결과 TiO2 혼입 샘플에서 더 많은 C-S-H의 생성량이 관찰되었으며, 이는 TiO2 혼입 시멘트 페이스트의 28일 압축강도 증가에 영향을 미친 것으로 판단된다. SEM/EDS 분석결과 P-25, GST, NP-400 순으로 페이스트 샘플 표면에 더 많은 Ti 원소의 함량이 관찰되었지만, NOx 제거 성능은 P-25, NP-400, GST 순으로 우수한 것으로 확인되었다.

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

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • 제27권6호
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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.

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

  • 신형섭;이상걸;권순주
    • 한국세라믹학회지
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    • 제29권3호
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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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    • 제14권4호
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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.

Effect of rock mineralogy on mortar expansion

  • Karaman, Kadir;Bakhytzhan, Aknur
    • Geomechanics and Engineering
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    • 제20권3호
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    • pp.233-241
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    • 2020
  • Alkali-silica reaction (ASR) is among one of the most important damaging mechanisms in concrete, depending primarily on aggregates which contain reactive minerals. However, expansion in concrete may not directly relate to the reactive minerals. This study aims to investigate the influence of ASR and the expansion of mortar bars depending on aggregate type containing various components such as quartz, clay minerals (montmorillonite and kaolinite) and micas (muscovite and biotite). In this study, the accelerated mortar bar tests (AMBT) were performed in two conditions (mortar bars in the same and sole NaOH solutions). Petrographic thin section studies, X-ray diffraction (XRD) analysis (Rietveld method), scanning electron microscopy (SEM) and chemical analyses were carried out. This study showed that quartzite bars led to increase in expansion values of mortar bars in diabase-1 and andesite when these were in the same NaOH solution. However, three samples (basalt, quartzite and claystone) were found having ASR expansion based on the AMBT when the special molds were used for each sample. SEM study revealed that samples which exhibit highest expansions according to AMBT had a generally rough surface and acicular microstructures in or around the micro-cracks. Basalt and quartzite showed more variable in major oxides than those of other samples based on the chemical analyses, SEM studies and AMBT. This study revealed that the highest expansions were observed to source not only from reactive aggregates but also from alteration products (silicification, chloritization, sericitization and argillisation), phyllosilicates (muscovite, biotite and vermiculite) and clays (montmorillonite and kaolinite).

황산제일철과 암모니아수를 이용한 산화철 합성 (Synthesis of Iron Oxide Using Ferrous Sulfate and Ammonia Water)

  • 김삼중;엄태형;왕웨이;서동수
    • 한국재료학회지
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    • 제18권4호
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    • pp.218-221
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    • 2008
  • A $Fe(OH)_2$ suspension was prepared by mixing iron sulfate and a weak alkali ammonia solution. Following this, iron oxides were synthesized by passing pure oxygen through the suspension (oxidation). The effects of different reaction temperatures ($30^{\circ}C$, $50^{\circ}C$, $70^{\circ}C$) and equivalent ratios ($0.1{\sim}10.0$) on the formation of iron oxides were investigated. An equilibrium phase diagram was established by quantitative phase analysis of the iron oxides using the Rietveld method. The equilibrium phase diagram showed a large difference from the equilibrium phase diagram of Kiyama when the equivalent ratio was above 1, and single $Fe_3O_4$ phase only formed above an equivalent ratio 2 at all reaction temperatures. Kiyama synthesized iron oxide using iron sulfate and a strong alkali NaOH solution.

Hydrogen Storage Properties of Hydriding-Dehydriding Cycled Magnesium-Nickel-Iron Oxide Alloy

  • Song, Myoung Youp;Kwon, Sung Nam;Park, Hye Ryoung;Kim, Byoung-Goan
    • 대한금속재료학회지
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    • 제50권2호
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    • pp.171-175
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    • 2012
  • By measuring the absorbed hydrogen quantity as a function of the number of cycles, the cycling properties of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy were investigated. The absorbed hydrogen quantity decreased as the number of cycles increased. The $H_a$ value varied almost linearly with the number of cycles. The maintainability of absorbed hydrogen quantity at n=100 was 89.0% for the hydriding reaction time of 10 min. After the $150^{th}$ hydriding-dehydriding cycle, Mg, $Mg_2Ni$, $Mg(OH)_2$, MgO, and Fe were observed. The phases were analyzed by Rietveld analysis from the XRD patterns of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy after 150 hydriding-dehydriding cycles. The crystallite size and strain of Mg were then estimated with the Williamson-Hall technique.

Structural Characterization of the (TEX)$Sr_2Co_0.5Nb(Ta)_0.5O_4$(/TEX) and (TEX)$Sr_3CoNb(Ta)O_7$(/TEX)

  • 조한상;;류광현;유철현
    • Bulletin of the Korean Chemical Society
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    • 제21권7호
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    • pp.679-684
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    • 2000
  • The Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 compounds, both with Ruddlesden-Popper structures, have been synthesized by the ceramic method at $1150^{\circ}C$ under atmospheric pressure. The crystallographic structure of the compounds was assigned to the tetr agonal system with space group 14/mmm by X-ray diffraction(XRD) Rietveld refinement. The reduced lattice volume and lattice parameters increased as the Ta with 5d substitutes for the Nb with 4d in the compounds. The Co/Nb(Ta)O bond length has been determined by X-ray absorption spectroscopic(EXAFS/XANES) analysis and the XRD refinement. The CoO6,octahedra were tetragonally distorted by elongation of Co-O bond along the c-axis. The magnetic measurement shows the compounds Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 have paramagnetic properties and the Co ions with intermediate spin sates between high and low spins in D4h symmetry. All the compounds showed semiconducting behavior whose electrical conductivity increased with temperature up to 1000 K. The electrical conductiviy increased and the activation energy for the conduction decreased as the number of perovskite layers increased in the compounds with chemical formula An+1BnO3n+1.

Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구 (Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1))

  • 박일진;김철성
    • 한국자기학회지
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    • 제18권2호
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1)의 조성을 가지는 분말 시료를 sol-gel 법과 진공봉합 열처리를 이용하여 합성하였다. x선 회절기, $M\ddot{o}ssbauer$ 분광기를 이용하여 시료의 결정구조 및 Ga 이온의 점유도에 관하여 연구하였다. XRD측정결과 $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ (x=0, 1)의 결정구조는 Ia3d의 공간그룹을 갖는 cubic 구조이며, $Tb_2Bi_1Fe_5O_{12}$$Tb_2Bi_1Ga_1Fe_4O_{12}$의 격자상수 $a_0$는 각각 $12.497\AA$, $12.465\AA$으로 분석되었다. Rietveld 분석법을 이용하여 각 이온들이 점유하는 각각의 부격자 위치를 연구하였다. $Tb_2Bi_1Ga_1Fe_4O_{12}$ 시료의 분석결과, Tb, Bi 이온은 24c 자리에, Fe 이온은 24d, 16a 자리를 점유하였으며, 비자성 이온인 Ga 이온은 모두 16a 자리를 점유하는 것으로 분석되었다. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1)의 미시적인 자기구조를 분석하기 위해 시료들의 $M\ddot{o}ssbauer$스펙트럼을 측정하였다. 상온에서의 $M\ddot{o}ssbauer$스펙트럼 측정결과 철 이온들의 흡수 면적비는 $Tb_2Bi_1Fe_5O_{12}$의 경우 24d와 16a자리에서 각각 60.8%, 39.2%로, $Tb_2Bi_1Ga_1Fe_4O_{12}$의 경우 24d와 16a자리에서 각각 74.7%, 25.3%로 분석되었다. 철 이온들의 흡수 면적비 분석을 통해 비자성이온인 Ga은 모두 16a 자리를 점유하는 것을 알 수 있었다.