• 제목/요약/키워드: X-ray Structure Analysis

검색결과 1,125건 처리시간 0.029초

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
    • /
    • 제14권4호
    • /
    • pp.161-164
    • /
    • 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.

Synthesis and Characteristics of the Organic Layered Structure Material of $(C_4H_9NH_3)_2Fe_xPb_1-xCl_4$

  • 정수진;인리주;오응주;조웅인;김규홍;요철현
    • Bulletin of the Korean Chemical Society
    • /
    • 제22권7호
    • /
    • pp.703-708
    • /
    • 2001
  • K2NiF4-type organic-based perovskites of the (C4H9NH3)2FexPb1-xCl4 (x=0.00, 0.25, 0.50, and 0.75) system have been synthesized using a low-temperatu re solution method under a flowing argon gas. When stoichiometric butylamine, iron chloride, and lead chloride are mixed, a yellow solution are obtained from slow cooling of 90 to -10 $^{\circ}C.$ The final product is a plate-like yellow crystal. The X-ray crystallographic analysis has been carried out using XRD in the range of $5^{\circ}{\leq}$ 2${\theta}$ ${\leq}80^{\circ}.$ The local symmetry around the absorbing Pb atom of the samples has been determined by the EXAFS spectroscopic study. The crystals assign to orthorhombic system by the XRD analysis. The FT-IR spectra are analyzed in the range of 600 to 3300 cm-1 . DSC and TGA are measured to detect thermal stability between 30 and 300 $^{\circ}C.$ Two endothermic peaks are detected in all samples. The electrical conductivity has been measured using the four-probes technique for the (C4H9NH3)2FexPb1-xCl4 system in 300-460 K. Photoluminescence phenomenon was also investigated at room-temperature.

Irradiation enduced In-plane magnetization in Fe/MgO/Fe/Co multilayers

  • Singh, Jitendra Pal;Lim, Weon Cheol;Song, Jonghan;Kim, Jaeyeoul;Asokan, K.;Chae, Keun Hwa
    • 한국진공학회:학술대회논문집
    • /
    • 한국진공학회 2015년도 제49회 하계 정기학술대회 초록집
    • /
    • pp.188.1-188.1
    • /
    • 2015
  • For present investigation Fe/MgO/Fe/Co multilayer stack is grown on Si substrate using e-beam evaporation in ultrahigh vacuum. This stack is irradiated perpendicularly by 120 MeV $Ag^{8+}$ at different fluences ranging from $1{\times}10^{11}$ to $1{\times}10^{13}ions/cm^2$ in high vacuum using 15UD Pelletron Accelerator at Inter University Accelerator Centre, New Delhi. Magnetic measurements carried out on pre and post irradiated stacks show significant changes in the shape of perpendicular hysteresis which is relevant with previous observation of re-orientation of magnetic moment along the direction of ion trajectory. However increase in plane squareness may be due to the modification of interface structure of stacks. X-ray reflectivity measurements show onset of interface roughness and interface mixing. X-ray diffraction measurements carried out using synchrotron radiation shows amorphous nature of MgO and Co layer in the stack. Peak corresponding body centered Fe [JCPDS-06-0696] is observed in X-ray diffraction pattern of pre and post irradiated stacks. Peak broadening shows granular nature of Fe layer. Estimated crystallite size is $22{\pm}1nm$ for pre-irradiated stack. Crystallite size first increases with irradiation then decreases. Structural quality of these stacks was further studied using transmission electron microscopic measurements. Thickness from these measurements are 54, 36, 23, 58 and 3 nm respectively for MgO, Fe, MgO, Fe+Co and Au layers in the stack. These measurements envisage poor crystallinity of different layers. Interfaces are not clear which indicate mixing at interface. With increase fluence mixing and diffusion was increased in the stack. X-ray absorption spectroscopic measurements carried out on these stacks show changes of Fe valence state after irradiation along with change of O(2p)-metal (3d) hybridized state. Valence state change predicts oxide formation at interface which causes enhanced in-plane magnetization.

  • PDF

영월 하송리 출토 금속유물 보존처리 및 제작기법 연구 (Production Techniques for the Metal Artifacts Excavated in Hasong-ri, Yeongwol and Their Conservation Treatment)

  • 이병훈;고형순;김수기
    • 박물관보존과학
    • /
    • 제21권
    • /
    • pp.53-66
    • /
    • 2019
  • 본 연구는 강원도 영월 하송리 유적에서 출토된 금속유물의 보존처리 과정과 표면성분분석 결과를 제시하였다. 금동소형풍탁 1점, 풍설 2점, 호리병 형태 소형 청동병 1점을 대상으로 XRF를 이용한 표면 성분분석을 진행하였고, 호리병 형태 소형청동병은 X-ray를 통한 내부구조관찰을 실시하였다. 금동소형풍탁과 풍설은 같은 위치에서 출토되었으나, 금동소형풍탁은 도금층이 확인되는데 반해, 풍설은 부식층이 표면에 고착되어 가시적으로 확인되지 않았다. 분석결과 금동소형풍탁은 Cu-Sn-Pb 3원계 합금 청동소지에 Au를 수은 아말감으로 도금하여 제작하였음을 확인하였다. 풍설은 소지가 구리이며, 소량의 금성분이 검출되었다, 호리병 형태 소형 청동병은 형태적으로 비슷한 고려시대 화폐인 은병(銀甁)인지 여부를 확인하고자 표면 성분분석과 함께 X-ray 촬영을 실시하였다. X-ray 촬영 결과 저부의 가운데 부분에 작은 구멍을 막았던 것으로 보이는 흔적이 확인되었으며, 전체적인 표면분석 결과에서는 은이 검출되지 않아 은병이 아닌 청동유물임을 알 수 있었다.

미소 초점 X선 CT를 이용한 암석 내 공극의 분포 및 공극률 분석 (Analysis of Porosity and Distribution of Pores in Rocks by Micro Focus X-Ray CT)

  • 정교철
    • 지질공학
    • /
    • 제20권4호
    • /
    • pp.461-465
    • /
    • 2010
  • 암석에서의 풍화 및 투수성은 방사성폐기물 지하동굴처분 및 암반구조물의 안정성 확보 및 장기적 관리측면에서 매우 중요한 역할을 한다. 이들 암석의 풍화 및 투수성은 암석의 내 구조 특성에 따라 크게 영향을 받는다. 즉 암석 내부의 공극, 미소 크랙 등의 양적 정도에 의해 풍화가 빨리 진행되기도 한다. 또한 암석 내부구조의 양적 평가는 그 암석의 풍화 정도를 정량적으로 평가할 수 있는 수단이 되기도 한다. 따라서 암석의 내부구조를 3치원적으로 정확하게 파악한다는 것은 암반구조물의 장기적 관리 측면에서 매우 중요하다고 하겠다. 이 연구는 국내 신선한 화강암과 풍화된 화강암을 대상으로 X선 CT촬영을 실시하여 3차원으로 공극의 분포를 분석하였다. 분석 결과는 암석 내부의 공극의 분포와 공극률을 잘 표현하고 있다.

Mechanistic investigations on emission characteristics from g-C3N4, gC3N4@Pt and g-C3N4@Ag nanostructures using X-ray absorption spectroscopy

  • Sharma, Aditya;Varshney, Mayora;Chae, Keun Hwa;Won, Sung Ok
    • Current Applied Physics
    • /
    • 제18권11호
    • /
    • pp.1458-1464
    • /
    • 2018
  • An improved method for the preparation of g-$C_3N_4$ is described. Currently, heating (> $400^{\circ}C$) of urea is the common method used for preparing the g-$C_3N_4$. We have found that sonication of melamine in $HNO_3$ solution, followed by washing with anhydrous ethanol, not only reduce the crystallite size of g-$C_3N_4$ but also facilitate intriguing electronic structure and photoluminescence (PL) properties. Moreover, loading of metal (Pt and Ag) nanoparticles, by applying the borohydride reduction method, has resulted in multicolor-emission from g-$C_3N_4$. With the help of PL spectra and local electronic structure study, at C K-edge, N K-edge, Pt L-edge and Ag K-edge by X-ray absorption spectroscopy (XAS), a precise mechanism of tunable luminescence is established. The PL mechanism ascribes the amendments in the transitions, via defect and/or metal states assimilation, between the ${\pi}^*$ states of tris-triazine ring of g-$C_3N_4$ and lone pair states of nitride. It is evidenced that interaction between the C/N 2p and metal 4d/5d orbitals of Ag/Pt has manifested a net detraction in the ${\delta}^*{\rightarrow}LP$ transitions and enhancement in the ${\pi}^*{\rightarrow}LP$ and ${\pi}^*{\rightarrow}{\pi}$ transitions, leading to broad PL spectra from g-$C_3N_4$ organic semiconductor compound.

Nd2XCd2-3XSiO4 (0.01≤X≤0.21) 고용체의 합성과 구조 규명 (Synthesis, Structure and Characterization of Nd2XCd2-3XSiO4 (0.01≤X≤0.21) Solid-Solutions)

  • Ramesh, S.;Das, B.B.
    • 대한화학회지
    • /
    • 제55권3호
    • /
    • pp.502-508
    • /
    • 2011
  • [ $Nd_{2x}Cd_{2-3x}SiO_4$ ]($0.01{\leq}x{\leq}0.21$) [S1-S3: x=0.01, 0.11 and 0.21] 고용체를 졸-겔 방법을 통해 합성하였다. X선 분말회절(XRD) 측정은 $P2_1$/m 공간군의 단사정계를 보여준다. 평균 결정 크기는 20-45 nm이다. 주사전자현미경(SEM)으로 살펴본 모양은 구형의 특성을 보인다. 에너지 분산 X 선 분광기(EDS) 결과로부터 모든 구성 원소의 존재를 확인하였다. ~750 nm에서의 흡수 밴드는 $Nd^{3+}$ 이온의 $^4I_{9/2}{\rightarrow}^4F_{7/2}+^4S_{3/2}$ 전이에 기인한다. 10, 40, 77, 300 K에서 S1-S3의 전자 상자성 공명 (EPR) 선모양은 $Nd^{3+}$ 이온의 빠른 스핀 격자 이완에 기인하는 폭이 넓은 구분되지 않은 등방성의 선모양을 보여준다.

Synthesis and structure analysis of the bis(dicyclohexylammonium) chromate dihydrate complex, [(C6H11)2NH2]2[CrO4]·2H2O

  • Kim, Chong-Hyeak;Moon, Hyoung-Sil;Lee, Sueg-Geun
    • 분석과학
    • /
    • 제20권5호
    • /
    • pp.448-451
    • /
    • 2007
  • A new bis(dicyclohexylammonium) chromate dihydrate complex, $[(C_6H_{11})_2NH_2]_2[CrO_4]{\cdot}2H_2O$, (I), has been synthesized and its structure analyzed by FT-IR, EDS, elemental analysis, ICP-AES, and single crystal X-ray diffraction methods. The Cr(VI) complex (I) is tetragonal system, I${\bar{4}}$2d space group with a = 12.5196(1), b = 12.5196(1), c = $17.3796(3){\AA}$, a = ${\beta}$ = ${\gamma}$ = $90^{\circ}$, V = $2724.09(6){\AA}^3$, Z = 4. The crystal structure of complex (I) consists of tetrahedral chromate $[CrO_4]^{2-}$ anion, two organic dicyclohexylammonium $[(C_6H_{11})_2NH_2]^+$ cations and two lattice water molecules. The chromate anion and protonated dicyclohexylammonium cation is mainly constructed through the ionic bond. The cyclohexylammonium rings of the dicyclohexylammonium cation take the chair form and vertical configuration with each other. The N-H${\cdot}$O and O-H${\cdot}$O hydrogen bond networks between the $N_{dicyclohexylammonium}$, $O_{water}$ and $O_{chromate}$ atom lead to self-assembled molecular conformation and stabilize the crystal structure.

Structural analysis of sialyltransferase PM0188 from Pasteurella multocida complexed with donor analogue and acceptor sugar

  • Kim, Dong-Uk;Yoo, Ji-Ho;Lee, Yong-Joo;Kim, Kwan-Soo;Cho, Hyun-Soo
    • BMB Reports
    • /
    • 제41권1호
    • /
    • pp.48-54
    • /
    • 2008
  • PM0188 is a newly identified sialyltransferase from P. multocida which transfers sialic acid from cytidine 5'-monophosphonuraminic acid (CMP-NeuAc) to an acceptor sugar. Although sialyltransferases are involved in important biological functions like cell-cell recognition, cell differentiation and receptor-ligand interactions, little is known about their catalytic mechanism. Here, we report the X-ray crystal structures of PM0188 in the presence of an acceptor sugar and a donor sugar analogue, revealing the precise mechanism of sialic acid transfer. Site-directed mutagenesis, kinetic assays, and structural analysis show that Asp141, His311, Glu338, Ser355 and Ser356 are important catalytic residues; Asp141 is especially crucial as it acts as a general base. These complex structures provide insights into the mechanism of sialyltransferases and the structure-based design of specific inhibitors.

상수관로 내부 오염물질의 물리화학적 특성 분석 (A study of physical and chemical properties of internal accumulated material in water mains)

  • 배철호;최두용;이두진;김도환
    • 상하수도학회지
    • /
    • 제28권5호
    • /
    • pp.589-600
    • /
    • 2014
  • Tuberculation and slime accumulated in water mains play an important role in modifying water quality of drinking water. Therefore, in this study, it was investigated that what materials were accumulated, and what components were included in the tuberculation and slime of water mains. The Various tuberculation and slime sample were collected from the 12 water mains to analyze their physical and chemical properties and crystal structure. As a analysis method, VSS(Volatile suspended solid), SEM(scanning electron microscope), EDS(Energy Dispersive X-ray spectroscope), ICP(Inductively Coupled Plasma Mass Spectrometer) and XRD(X-Ray Diffractomete) were used. The results of analysis on the samples, the representative materials were verified such as iron corrosion products, the fine sand particles generated during backwash, fine particles of activated carbon, aluminum used in coagulation process, and manganese included in raw water.