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SYNCHROTRON RADIATION CHARACTERIZATION OF COBALT NANOPARTICLES FORMED BY ION IMPLANTATION 离子注入形成的钴纳米粒子的同步辐射特性
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000203
D. Sprouster, R. Giulian, P. Kluth, L. Araujo, G. Foran, D. Cookson, M. Ridgway
Ion implantation of Co into silica layers and subsequent thermal annealing were used to form Co nanoparticles. Structural characterization was performed using X-ray Absorption Spectroscopy and Small Angle X-ray Scattering to determine, respectively, the local atomic structure and size distribution of the Co nanoparticles as a function of annealing temperature. For decreasing nanoparticle size, a bond-length contraction, an increase in Debye–Waller factor and a reduction in coordination number were observed. The bond-length contraction was related to the capillary pressure in the nanoparticles while an increase in Debye–Waller factor reflected an increase in disorder attributed to the high surface-area-to-volume ratio of small nanoparticles. X-ray Absorption Near Edge Structure spectroscopy revealed that the annealing conditions had a significant effect on the nanoparticle crystal structure and oxidised Co fraction.
将Co离子注入到二氧化硅层中,然后进行热退火,形成Co纳米颗粒。利用x射线吸收光谱和小角x射线散射进行结构表征,分别确定Co纳米粒子的局部原子结构和尺寸分布随退火温度的变化规律。随着纳米颗粒尺寸的减小,观察到键长收缩,德拜-沃勒因子增加和配位数降低。键长收缩与纳米颗粒的毛细管压力有关,而Debye-Waller因子的增加反映了小颗粒的高表面积体积比导致的无序性增加。x射线吸收近边结构光谱显示,退火条件对纳米颗粒的晶体结构和氧化Co分数有显著影响。
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引用次数: 0
ANGLE-DEPENDENT MEASUREMENTS OF ELONGATED PLATINUM NANOCRYSTALS USING SMALL ANGLE X-RAY SCATTERING 使用小角度x射线散射的细长铂纳米晶体的角度依赖性测量
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000239
R. Giulian, P. Kluth, D. Sprouster, L. Araujo, D. Llewellyn, A. Byrne, D. Cookson, M. Ridgway
Elongated Pt nanocrystals (NCs) formed in SiO2 by ion implantation, thermal annealing and swift heavy ion irradiation (SHII) were analyzed by small angle X-ray scattering (SAXS) and transmission electron microscopy (TEM) measurements. Transmission SAXS measurements were performed in samples aligned at different angles relative to the photon beam resulting in nonisotropic scattering and thus enabling the three-dimensional analysis of the NCs. Selected angular sectors of the detector were integrated and analyzed separately, leading to the individual evaluation of both the major and minor dimensions of the rod-shaped NCs. This method enables the use of well-established spherical models for the SAXS data analysis and yielded good agreement with TEM results. Corrections to the amplitude of the SAXS diameter distributions to overcome the disparities between the spherical models and the nonspherical particles are also presented.
采用小角x射线散射(SAXS)和透射电子显微镜(TEM)对离子注入、热退火和快速重离子辐照(SHII)在SiO2中形成的细长Pt纳米晶体(NCs)进行了分析。透射SAXS测量是在相对于光子束以不同角度排列的样品中进行的,导致非各向同性散射,从而能够对nc进行三维分析。将探测器选定的角扇区进行集成和单独分析,从而对棒状nc的主要尺寸和次要尺寸进行单独评估。该方法可以使用成熟的球面模型进行SAXS数据分析,并与TEM结果很好地吻合。对SAXS直径分布的振幅进行修正,以克服球形模型与非球形模型之间的差异。
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引用次数: 1
ANISOTROPY AND STRUCTURAL CHARACTERIZATION OF Co/Pd MULTILAYER THIN FILMS 钴/钯多层薄膜的各向异性及结构表征
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000215
P. Vahdani, A. S. Rozatian, J. Amighian
In this paper, magnetic and structural properties as well as the interface morphology of a series of sputtered Co/Pd multilayer thin films have been investigated. Interface morphology has been studied from grazing incidence specular and off-specular X-ray measurements using synchrotron radiation. High-angle X-ray diffraction measurements indicate a modulated structure which is strongly textured grown along (111) direction. The relation between intensity and the number of bilayers for different peaks of high-angle X-ray diffraction measurements has been investigated and compared to the grazing incidence X-ray scattering results. Vibrating sample magnetometer measurements have shown perpendicular magnetic anisotropy for all samples with Keff reaching highest value for those samples with highest fractal parameter.
本文研究了一系列溅射Co/Pd多层薄膜的磁性、结构性能和界面形貌。利用同步辐射从掠入射镜面和非镜面x射线测量中研究了界面形貌。高角度x射线衍射测量表明,这是一种沿(111)方向生长的强烈织构的调制结构。研究了高角x射线衍射测量中不同峰的强度与双层数的关系,并与掠入射x射线散射结果进行了比较。振动样品磁强计测量结果表明,所有样品的磁各向异性均为垂直,分形参数最大的样品的Keff值最大。
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引用次数: 0
Nondestructive three-dimensional x-ray diffraction imaging of nanoscale particles 纳米级粒子的无损三维x射线衍射成像
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000276
A. Nikulin, R. Dilanian, B. M. Gable, B. C. Muddle, J. Hester, T. Ishikawa, P. Yang, H. Moser
We report a novel approach to X-ray diffraction data analysis for nondestructive determination of the shape of nanoscale particles and clusters in three dimensions with a spatial resolution of a few nanometers. The advantage of the proposed approach is that it does not require a coherent X-ray source and therefore is suitable for almost any synchrotron radiation beamline and many laboratory sources. The technique is insensitive to the coherence of the X-rays, and 3D reconstruction of a modal image is possible without tomographic synthesis, rendering the approach suitable for laboratory facilities. Successful application of the technique to the characterization of nanoparticulate in a range of dispersed-phase nanocomposite structures illustrates this novel approach.
我们报告了一种新的x射线衍射数据分析方法,用于在三维空间分辨率为几纳米的情况下无损测定纳米级颗粒和团簇的形状。所提出的方法的优点是它不需要相干x射线源,因此适用于几乎任何同步辐射光束线和许多实验室源。该技术对x射线的相干性不敏感,并且无需层析合成即可实现模态图像的3D重建,因此该方法适用于实验室设施。该技术在一系列分散相纳米复合材料结构中纳米颗粒表征的成功应用说明了这种新方法。
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引用次数: 0
INTERACTIONS OF COPPER AND ZINC IN MCM-41 McM-41中铜和锌的相互作用
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000185
Hsin-Liang Huang, H. -. Wang, H. Wang, Yu-Ling Wei
Speciation of copper and zinc (1:1) in MCM-41 has been studied by X-ray absorption near edge structural (XANES) and X-ray absorption fine structural (EXAFS) spectroscopies in the present work. The least-square fitted XANES spectra show that Cu(II) and Zn(II) are the major copper and zinc species, respectively in the channels of MCM-41 during calcination at 573–1173 K. The EXAFS data indicate that copper in MCM-41 possesses a Cu–O bond distance of 1.97 A with a coordination number (CN) of 3.4. During calcination at 573–1173 K, about 3.8–4.2 nearest oxygen atoms are bonded to the central copper atoms with Cu–O bond distances of 1.95–1.96 A in MCM-41. A small amount of Cu–Zn alloy may be formed during calcination. Existence of Zn–O)–Si (3.05–3.11 A) with CNs of 1.7–2.3 is also observed by EXAFS, suggesting an interaction between zinc and the framework SiO2 of MCM-41 during calcination.
本文利用x射线吸收近边结构(XANES)和x射线吸收精细结构(EXAFS)光谱研究了MCM-41中铜和锌(1:1)的形态。最小二乘拟合XANES光谱结果表明,在573 ~ 1173 K的高温下,MCM-41通道中的铜和锌分别以Cu(II)和Zn(II)为主。EXAFS数据表明MCM-41中铜的Cu-O键距为1.97 a,配位数(CN)为3.4。在573 ~ 1173 K的温度下,MCM-41中有3.8 ~ 4.2个最近的氧原子与中心铜原子成键,Cu-O键距为1.95 ~ 1.96 A。在煅烧过程中会形成少量的Cu-Zn合金。EXAFS还观察到CNs为1.7-2.3的Zn-O) -Si (3.05-3.11 A)的存在,表明MCM-41在煅烧过程中锌与骨架SiO2发生了相互作用。
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引用次数: 0
MEASUREMENT OF YOUNG'S MODULUS AND POISSON'S RATIO OF THIN FILMS BY SYNCHROTRON X-RAY DIFFRACTION 同步x射线衍射法测量薄膜的杨氏模量和泊松比
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000288
Y. H. Yu, M. Lai, L. Lu, G. Zheng
A new experimental method for determining elastic constants of thin films is proposed. The curvatures of the single crystal substrates before and after depositing thin film are first measured using high-resolution X-ray rocking curve technique with high quality monochromatic and high intensity synchrotron radiation. The residual stress in the film is then calculated from the change in substrate curvature based on the well-known modified Stoney's equation. The formulae for calculating thin film's Young's modulus and Poisson's ratio are deduced based on measured residual stress and the lattice spacing dψ versus sin2ψ curves of the film before and after an unknown mechanical loading. LaNiO3 film grown on single crystal silicon substrate using pulsed laser deposition is employed to demonstrate the measurement method.
提出了一种测定薄膜弹性常数的新实验方法。采用高分辨率x射线摇摆曲线技术,在高质量单色和高强度同步辐射下,测量了单晶衬底沉积薄膜前后的曲率。然后根据著名的修正Stoney方程,从衬底曲率的变化计算薄膜中的残余应力。根据薄膜在未知机械载荷前后的残余应力和晶格间距dψ与sin2ψ曲线,推导出薄膜的杨氏模量和泊松比的计算公式。采用脉冲激光沉积法在单晶硅衬底上生长LaNiO3薄膜,演示了测量方法。
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引用次数: 1
PROPERTIES OF Ge NANOCRYSTALS DETERMINED BY EXAFS AND SAXS 用EXAFS和SAXS测定锗纳米晶的性质
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000227
L. Araujo, R. Giulian, P. Kluth, B. Johannessen, D. Cookson, G. Foran, M. Ridgway
We report on the atomic level structural properties of Ge nanocrystals (Ge NCs) grown by ion implantation and thermal annealing. The synchrotron-based techniques of extended X-ray absorption fine structure (EXAFS) spectroscopy and small angle X-ray scattering (SAXS) were applied to characterize the Ge NCs. Four different size distributions of Ge NCs were produced in amorphous SiO2 matrices, with mean diameters ranging from 4.0 to 9.0 nm as verified by SAXS measurements. The decrease in size, or increase in surface-to-volume ratio, for the NCs leads to a decrease in the crystalline-like features in the X-ray absorption near-edge structure (XANES) and EXAFS regions of the X-ray absorption spectra. It also yields a decrease in coordination number and an increase in mean interatomic distance, structural disorder, and asymmetry of the interatomic distance distribution. By comparison with bulk standards, the NCs are described as a combination of crystalline Ge core and surrounding amorphous Ge-like surface layer.
本文报道了离子注入和热退火法制备的锗纳米晶体的原子级结构特性。采用同步加速器扩展x射线吸收精细结构(EXAFS)光谱和小角x射线散射(SAXS)技术对锗纳米粒子进行了表征。在无定形SiO2基体中制备了四种不同尺寸分布的Ge NCs,经SAXS测量证实,其平均直径在4.0 ~ 9.0 nm之间。纳米颗粒尺寸的减小或表面体积比的增加导致x射线吸收光谱近边结构(XANES)和EXAFS区域的类晶特征减少。配位数减少,平均原子间距离增加,结构紊乱,原子间距离分布不对称。与体标准相比,nc被描述为结晶Ge芯和周围非晶类Ge表面层的组合。
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引用次数: 1
PRESENT STATUS AND FUTURE PLAN OF COMPACT SR RING HiSOR 紧凑型SR环历史机的现状与未来规划
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000161
T. Hori, A. Miyamoto, K. Goto, H. Tsutsui
Hiroshima Synchrotron Radiation Center (HSRC) is a common facility for research and education in the field of synchrotron radiation science in Japan. The major role of the facility is to promote nationwide SR research activities in materials science, especially in solid state physics, and education in the related fields simultaneously. HiSOR is a compact synchrotron radiation source of HSRC constructed in 1996 as a typical VUV — soft X-ray source (0.87 keV critical photon energy) similar to Helios in Singapore. Because of a compact racetrack-type ring, its natural emittance 400π nm · rad is not so small as the other standard-sized rings. There are two undulators, one linear for 26–300 eV range and the other helical/linear for 4–40 eV. The most outstanding feature of the facility lies in the good combination with beamlines to attain high-resolution (below 1 meV) for photoemission spectroscopy. It is routinely operated from 09:00 to 20:00 on weekdays at the stored current starting from 350 mA with 8 h lifetime at 300 mA. HiSOR has been running over 10 years, thus, it is time to think about the future improvements of the facility. The motivation is to pursue the leading position in the field of materials science (solid state physics) using SR for high-resolution photoemission spectroscopy. Some candidates for the upgraded HiSOR are presented.
广岛同步辐射中心(HSRC)是日本同步辐射科学领域的研究和教育的公共设施。该机构的主要作用是促进全国材料科学,特别是固体物理领域的SR研究活动,同时促进相关领域的教育。HiSOR是HSRC于1996年建成的一个紧凑型同步辐射源,是一个典型的VUV -软x射线源(0.87 keV临界光子能量),类似于新加坡的Helios。赛道型环结构紧凑,其自然发射度400π nm·rad不小于其他标准尺寸环。有两个波动器,一个线性26-300 eV范围和另一个螺旋/线性4-40 eV。该设备最突出的特点在于与光束线的良好结合,以获得高分辨率(低于1mev)的光电发射光谱。正常工作时间为工作日09:00 - 20:00,存储电流为350毫安,300毫安时寿命为8小时。HiSOR已经运行了10多年,因此,是时候考虑未来设施的改进了。其动机是追求在材料科学(固体物理)领域的领先地位,利用SR进行高分辨率光电发射光谱。提出了一些升级后的候选HiSOR。
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引用次数: 0
IN SITU TIME RESOLVED LAUE DIFFRACTION DURING MICRO-COMPRESSION EXPERIMENTS 微压缩实验中现场时间分辨劳厄衍射
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000252
R. Maaß, S. Petegem, H. Swygenhoven, D. Grolimund, P. Derlet, C. Volkert
We present in situ and ex situ Laue micro-diffraction experiments on micron-sized single crystal pillars. We show that the focused ion beam technique introduces measurable damage in Si pillars. The dynamics of the Laue patterns of Au pillars demonstrate the occurrence of crystal rotation and strengthening is explained by plasticity starting on a slip system that is geometrically not predicted but selected because of the character of the pre-existing strain gradient.
本文对微米级单晶柱进行了原位和非原位劳厄微衍射实验。我们证明了聚焦离子束技术在硅柱中引入了可测量的损伤。金柱的劳厄模式的动力学表明,晶体旋转和强化的发生是由塑性开始的滑移系统来解释的,这种滑移系统在几何上是不可预测的,但由于预先存在的应变梯度的特征而被选择。
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引用次数: 0
SYNCHROTRON RADIATION PHOTOELECTRON STUDY OF HEUSLER-TYPE Fe2VAl-BASED ALLOYS heusler型fe2val基合金的同步辐射光电子研究
Pub Date : 2008-12-01 DOI: 10.1142/S1793617908000148
K. Soda, Hidetoshi Miyazaki, Koji Yamamoto, T. Mochizuki, M. Inukai, Masahiko Kato, S. Yagi, Y. Nishino
The electronic structures of Heusler-type Fe2VAl-based alloys, n-type thermoelectric alloys Fe2VAl1-zXz(X = Si, Ge) and p-type one Fe2(V1-yTiy)Al, have been investigated by photoelectron spectroscopy with use of synchrotron radiation as an excitation photon source. Observed valence-band spectra of Fe2VAl agree quite well with the predicted density of states with a sharp pseudogap across the Fermi energy EF. Small substitution in Fe2VAl1-zXz and Fe2(V1-yTiy)Al reveals a rigid-band-like energy shift of the valence band, although the observed shift is smaller than expected in the rigid band model. Further substitution causes the modification of the electronic structure near EF and the appearance of mid-pseudogap states. However, the dependence of the thermoelectric properties of these alloys on substitution can be qualitatively explained by the observed change in the electronic structure near EF.
利用同步辐射作为激发光子源,用光电子能谱研究了heusler型fe2val基合金、n型Fe2VAl1-zXz(X = Si, Ge)热电合金和p型Fe2(V1-yTiy)Al热电合金的电子结构。观测到的Fe2VAl的价带光谱与预测的在费米能量EF上有明显赝隙的态密度吻合得很好。Fe2VAl1-zXz和Fe2(V1-yTiy)Al中的小取代揭示了价带的刚性带式能量转移,尽管观察到的转移比刚性带模型中的预期要小。进一步的取代导致EF附近电子结构的改变和中赝隙态的出现。然而,这些合金的热电性能对取代的依赖可以通过观察到的EF附近电子结构的变化来定性地解释。
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引用次数: 6
期刊
Advances in Synchrotron Radiation
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