An X‐ray Raman spectrometer for EXAFS studies on minerals: bent Laue spectrometer with 20 keV X‐rays

An X‐ray Raman spectrometer for studies of local structures in minerals is discussed. Contrary to widely adopted back‐scattering spectrometers using ≤10 keV X‐rays, a spectrometer utilizing ～20 keV X‐rays and a bent Laue analyzer is proposed. The 20 keV photons penetrate mineral samples much more deeply than 10 keV photons, so that high intensity is obtained owing to an enhancement of the scattering volume. Furthermore, a bent Laue analyzer provides a wide band‐pass and a high reflectivity, leading to a much enhanced integrated intensity. A prototype spectrometer has been constructed and performance tests carried out. The oxygen K‐edge in SiO₂ glass and crystal (α‐quartz) has been measured with energy resolutions of 4 eV (EXAFS mode) and 1.3 eV (XANES mode). Unlike methods previously adopted, it is proposed to determine the pre‐edge curve based on a theoretical Compton profile and a Monte Carlo multiple‐scattering simulation before extracting EXAFS features. It is shown that the obtained EXAFS features are reproduced fairly well by a cluster model with a minimal set of fitting parameters. The spectrometer and the data processing proposed here are readily applicable to high‐pressure studies.     

An EXAFS study of interionic distances in complex lanthanide oxides

When the smaller vanadium ion is substituted for niobium in NdNbO₄, the volume of the unit cell is almost unchanged; in the lanthanum and cerium counterparts the volume actually increases. In order to understand these phenomena we have employed the technique of extended x-ray absorption fine structure (EXAFS) to determine all of the near neighbor anion-cation distances in the series of mixed-B-ion oxides, NdNb_1?xV_xO₄, including the end-member compounds, NdNbO₄ and NdVO₄. We find that the average Nb-O, V-O and Nd-O interionic distances in the mixed compounds closely resemble the distances exhibited in the corresponding end-member compounds, but there are large variances associated with these averages. We take this to mean that, while crystal symmetry is not broken by the substitution of the smaller V⁵⁺ ion, there are substantial local distortions in bond lengths and angles in order to meet the ion-size requirements of immediate neighbors.     

An EXAFS spectroscopic study of Am(III) complexation with lactate

The pH dependence (1–7) of Am(III) complexation with lactate in aqueous solution is studied using extended X‐ray absorption fine‐structure (EXAFS) spectroscopy. Structural data (coordination numbers, Am—O and Am—C distances) of the formed Am(III)–lactate species are determined from the raw k³‐weighted Am L_III‐edge EXAFS spectra. Between pH 1 and pH 6, Am(III) speciation shifts continuously towards complexed species with increasing pH. At higher pH, the amount of complexed species decreases due to formation of hydroxo species. The coordination numbers and distances (3.41–3.43 Å) of the coordinating carbon atoms clearly point out that lactate is bound `side‐on' to Am(III) through both the carboxylic and the α‐hydroxy function of lactate. The experimentally determined coordination numbers are compared with speciation calculations on the basis of tabulated thermodynamic stability constants. Both EXAFS data and thermodynamic modelling are in very good agreement. The EXAFS spectra are also analyzed by iterative transformation factor analysis to further verify the determined Am(III) speciation and the used structural model.     

Path degeneracy and EXAFS analysis of disordered materials

Analysis of EXAFS data measured on a material with a disordered local configuration environment around the absorbing atom can be challenging owing to the proliferation of photoelectron scattering paths that must be considered in the analysis. In the case where the absorbing atom exists in multiple inequivalent sites, the problem is compounded by having to consider each site separately. A method is proposed for automating the calculation of theory for inequivalent sites, then averaging the contributions from sufficiently similar scattering paths. With this approach, the complexity of implementing a successful fitting model on a highly disordered sample is reduced. As an example, an analysis of Ti K‐edge data on zirconolite, CaZrTi₂O₇, which has three inequivalent Ti sites, is presented.     

分光计调整实验中望远镜的调整技巧

在分光计的调整实验中,需要调整望远镜光轴与分光计的中心轴垂直,这一步是最关键、最困难的步骤．对于实验中经常出现的只能观察到一个“十”字叉丝反射像的问题,从光路上进行了详细的分析,提出了一个新的简单有效的调整方法,还给出了调整望远镜的完整流程图．     

真空紫外成像光谱仪在空间科学中的应用与展望

真空紫外成像光谱仪是空间科学研究中重要的数据获取工具,通过对不同天体目标真空紫外辐射的观测,可以反演出天体中主要物质的含量和变化规律,从而为空间天气、宇宙起源等许多前沿科学提供研究资料.分析了真空紫外成像光谱仪在空间科学研究中的优势,介绍了国外发展概况,列举了日地空间环境观测、地外行星体观测和宇宙空间观测三个应用领域中...     

The pH dependence of Am(III) complexation with acetate: an EXAFS study

The complexation of acetate with Am(III) is studied as a function of the pH (1–6) by extended X‐ray absorption fine‐structure (EXAFS) spectroscopy. The molecular structure of the Am(III)–acetate complexes (coordination numbers, oxygen and carbon distances) is determined from the raw k³‐weighted Am L_III‐edge EXAFS spectra. The results show a continuous shift of Am(III) speciation with increasing pH value towards the complexed species. Furthermore, it is verified that acetate coordinates in a bidentate coordination mode to Am(III) (Am—C distance: 2.82 ± 0.03 Å). The EXAFS data are analyzed by iterative transformation factor analysis to further verify the chemical speciation, which is calculated on the basis of thermodynamic constants, and the used structural model. The experimental results are in very good agreement with the thermodynamic modelling.     

光盘光谱仪的原理、制作及应用

根据光盘的分光作用,制作了利用光盘作为分光元件的光盘光谱仪.本文介绍了光盘光谱仪的原理、制作过程及性能测试.     

显微成像光谱仪技术的研究及应用

显微成像光谱仪技术是一种生物组织检测方法,目前广泛应用于生物医学检测和疑难病症分析,已成为组织检测领域的研究热点。论述了显微成像光谱仪各结构功能模块的工作原理及特点,并对其各主要技术指标进行了分析。介绍了目前的发展现状,并对所出现的多种显微成像光谱仪的技术方案及特点做了详细的总结。研究结果表明,显微成像光谱技术作为一种新的技术手段,必将在临床医学、生物学、材料学以及分析化学等领域得到广泛的应用。     

成像光谱技术的研究与发展

成像光谱技术是20世纪70年代末发展起来的一项新型航天航空遥感技术。综述了成像光谱技术的发展背景,在海洋、大气、植被、地质研究等领域的应用现状。介绍了成像光谱技术的几种主要分类、各种类型的特点以及国内外具有代表性的方案。提出了大孔径干涉型成像光谱仪的原理,并展示了攻关样机和实验数据。     

Pressure effects on EXAFS Debye-Waller factor and melting curve of solid krypton

The pressure effects on atomic mean-square displacement, extended X-ray absorption fine structure (EXAFS) Debye-Waller factor and melting temperature of solid krypton have been investigated in within the statistical moment method scheme in quantum statistical mechanics. By assuming the interaction between atoms can be described by Buckingham potential, we performed the numerical calculations for krypton up to pressure 120?GPa. Our calculations show that the atomic mean-square displacement and EXAFS Debye-Waller factor of krypton crystal depend strongly on pressure. They make the robust reduction of the EXAFS peak height. Our results are in good and reasonable agreements with available experimental data. This approach gives us a relatively simple method for qualitatively calculating high-pressure thermo-physical properties of materials. Moreover, it can be used to verify future high-pressure experimental and theoretical works.     

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介绍了为开展漏孔检测、氘-氦分辨性能及真空检漏技术等相关实验研究而进行的四极质谱计分析与测量系统的研制,描述了真空室结构、抽气设备的选型、测量仪器的选择及控制保护子系统工作方式。对系统进行了包括极限真空、残余气体质谱分析、漏放气率、质谱计性能等测试,结果表明本系统达到了设计要求。     

中子三轴谱仪的原理、技术与应用

中子作为一种具有独特性质的亚原子粒子,在很多研究领域都具有重要且无法替代的优势.中子三轴谱仪通过能量守恒和动量守恒原理就可以测量某一系统的弹性或非弹性散射性质,从而获得该系统的结构或动力学信息.中子三轴谱仪得名于其3个核心部分:单色器、样品和分析器,每一部分都可以独立转动.由于三轴谱仪在物理学尤其是凝聚态物理学研究中所发挥的重要作用,中国科学院物理研究所将联合中国原子能科学研究院,在后者新建成的中国先进研究堆搭建一台现代化的热中子三轴谱仪.文章结合该谱仪,介绍了中子三轴谱仪的基本原理、技术以及应用范围.     

窗扫型成像光谱仪数据处理及误差校正研究

窗扫型傅里叶变换成像光谱仪具有高光通量和无动镜等特点,同时也增加了数据处理的难度,需要对采集的原始干涉图进行重组。通过对其数据处理流程特点的分析,设计了一种归一化算法,对由干涉图重组时产生的误差进行了校正,并对在数据采集过程中干涉图的中心暗纹位置的采样误差进行了二次曲线拟合校正。整个数据处理过程实现了从干涉数据立方体到光谱数据立方体的变换。从理论分析和实验结果的比较中验证了误差校正方法的有效性。     

多通道软X射线Dante谱仪标定及实验

 介绍了用于阳加速器上Z箍缩内爆实验诊断的Dante谱仪的结构和通道配置,详细讨论了X射线二极管、掠入射平面反射镜和滤片等主要元器件的标定结果,分析了标定结果与理论计算发生偏差的原因,给出了喷气Z箍缩等离子体辐射的测量结果,X光辐射功率30～40 GW,能量约0.8 kJ,并与闪烁体光电管测量结果进行了比较,差异约20%。     

超高分辨率光电子能谱仪和超导电子态的直接观察

文章较系统地介绍了光电子能谱仪的基本原理和现有光电子能谱仪的问题．在此基础上介绍了激光超高分辨率光电子能谱仪的优点，它采用的是Nd：YVO4激光六次谐波输出作为激光光源．最后给出了使用这台分辨率达0．36meV的超高分辨率光电子能谱仪，在国际上首次直接观察到CeRu2化合物超导体在超导态时的电子聚集和超导能隙。     

EXAFS study of local atomic order about iodine in thyroxine,rat, human and sheep thyroids

Radioactive ¹²⁵I emits short‐range Auger electrons and represents a human health risk when incorporated in thyroglobulin of the thyroid. Quantitative evaluation of this risk can only be realised if local atomic order about iodine in the thyroid is known. Here, extended X‐ray absorption fine structure (EXAFS) has been used to probe the local structure about iodine in pure thyroid hormone, thyroxine. These data are consistent with a model where iodine is bound to a single iodinated carbon ring linked to an oxygen atom, similar to a previously published model for monoiodotyrosine, a major iodinated residue in thyroglobulin. Several structural models for the local environment of iodine from rat, human and sheep have been tested and these data are found to be compatible with a slightly modified environment with respect to that found for thyroxine. The best‐fit models include the following three components: (i) iodine covalently bonded to a tyrosine ring, as found for thyroxine; (ii) iodine bonded quasi‐covalently to a carbonyl ligand in partially filled (50%) sites; (iii) partially filled sites (50–40%) of carbonyl ligands, with oxygen at van der Waals distances from iodine. Advantages of using Fourier‐filtered EXAFS for complex crystal structures are discussed.     

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利用一套四极质谱气体分析与测试系统,开展MicroVision Plus四极质谱计的氦(He)、氘(D2)分辨性能实验。分别向分析室送入He和D2,记录质谱图,得到质量刻度和分辨率等信息。He+峰位为(4.0022±0.0006)amu;D2+峰位为(4.0246±0.0006)amu。在10-6～10-4Pa的分压范围,观察到He和D2的分辨率随其分压强的增大而减小。在10-7Pa-m3-s-1的He漏孔条件下,调节D2送气量,He+/D2+分压峰值比在10-1量级可以分辨出He。     

EXAFS analysis of Er sites in Er–O and Er–F co-doped crystalline Si

We present extended X-ray absorption fine structure (EXAFS) and photoluminescence (PL) analyses of Er–O and Er–F co-doped Si. Samples were prepared by multiple implants at 77 K of Er and co-dopant (O or F) ions resulting in the formation of a2 μm thick amorphous layer uniformly doped with 1×10¹⁹ Er/cm³ and 3×10¹⁹ O/cm³, 1×10²⁰ O/cm³ or 1×10²⁰ F/cm³. EXAFS measurements show that the local environment of the Er sites in the amorphous layers consists of 6 Si first neighbors. After epitaxial regrowth at 620°C for 3 h, Er is fully coordinated with 8 F ions in the Er–F samples, while Si and O ions are concomitantly present in the first shell of O co-doped samples. Post regrowth thermal treatments at 900°C leave the coordination unchanged in the Er+F, while the Er+O (ratio 1 : 10) doped samples present Er sites with a fully O coordinated shell with an average of 5 O atoms and 4 O atoms after 30 s and 12 h, respectively. We have also found that the fine structure and intensity of the high-resolution PL spectra are strongly dependent on the Er-impurity ratio and on thermal process parameters in the Er–O co-doped samples, while this is not observed for the F-doped samples. The most intense PL response at 15 K was obtained for the 1 : 3 E : O ratio, suggesting that an incomplete O shell around Er is particularly suitable for optical excitation.     

High pressure atomic structure of Zr–Cu metallic glass via EXAFS spectroscopy and molecular dynamics simulations

ABSTRACT

In this work, we use extended X-ray absorption fine structure (EXAFS) data collected using nano-polycrystalline diamond anvil cell to study the atomic arrangement in Zr–Cu metallic glass in high pressure (HP) conditions. To reveal the microscopic details of stress accommodation mechanism, we performed molecular dynamics (MD) simulations of the HP atomic arrangement. By comparing the experimental and the calculated Zr and Cu K-edge EXAFS signal we prove the realistic character of the computer simulations. A detailed geometrical analysis of the simulated atomic configurations shows that with increasing hydrostatic pressure the local structure of Zr–Cu amorphous alloy becomes gradually dominated by Cu-centred icosahedral structural motifs involving fivefold symmetry incompatible with crystalline ordering. The variation of the short-range order is attributed to preferential straining of mechanically soft bonds between zirconium atoms.