第三代同步辐射光源X射线相干性测量研究

随着高性能第三代同步辐射光源的建成开放,基于X射线相干特性的实验方法得到了快速发展和广泛应用.作为一个典型的例子,X射线相位衬度成像已经成为常规的X射线实验方法并向用户开放.相干散射、相干衍射成像、光子关联谱等X射线实验方法正日益受到重视,在高空间分辨、时间分辨等研究领域已显示出其独特的优越性.因此,研究和测量第三代同步辐射的空间相干特性对进一步发展这些新的实验方法具有重要意义.基于Talbot自成像原理成功测量了上海光源X射线成像线站发射的X射线的空间相干长度,并进而测得了相应光源的空间尺度.光子能量为33.2 keV时,测得的X射线光束垂直方向空间相干长度为8.84μm,对应的光源尺寸为23μm,测量结果与理论分析相符.     

Cultural heritage and archaeology materials studied by synchrotron spectroscopy and imaging

The use of synchrotron radiation techniques to study cultural heritage and archaeological materials has undergone a steep increase over the past 10–15 years. The range of materials studied is very broad and encompasses painting materials, stone, glass, ceramics, metals, cellulosic and wooden materials, and a cluster of organic-based materials, in phase with the diversity observed at archaeological sites, museums, historical buildings, etc. Main areas of investigation are: (1) the study of the alteration and corrosion processes, for which the unique non-destructive speciation capabilities of X-ray absorption have proved very beneficial, (2) the understanding of the technologies and identification of the raw materials used to produce archaeological artefacts and art objects and, to a lesser extent, (3) the investigation of current or novel stabilisation, conservation and restoration practices. In terms of the synchrotron methods used, the main focus so far has been on X-ray techniques, primarily X-ray fluorescence, absorption and diffraction, and Fourier-transform infrared spectroscopy. We review here the use of these techniques from recent works published in the field demonstrating the breadth of applications and future potential offered by third generation synchrotron techniques. New developments in imaging and advanced spectroscopy, included in the UV/visible and IR ranges, could even broaden the variety of materials studied, in particular by fostering more studies on organic and complex organic–inorganic mixtures, while new support activities at synchrotron facilities might facilitate transfer of knowledge between synchrotron specialists and users from archaeology and cultural heritage sciences.     

European research platform IPANEMA at the SOLEIL synchrotron for ancient and historical materials

IPANEMA, a research platform devoted to ancient and historical materials (archaeology, cultural heritage, palaeontology and past environments), is currently being set up at the synchrotron facility SOLEIL (Saint‐Aubin, France; SOLEIL opened to users in January 2008). The new platform is open to French, European and international users. The activities of the platform are centred on two main fields: increased support to synchrotron projects on ancient materials and methodological research. The IPANEMA team currently occupies temporary premises at SOLEIL, but the platform comprises construction of a new building that will comply with conservation and environmental standards and of a hard X‐ray imaging beamline today in its conceptual design phase, named PUMA. Since 2008, the team has supported synchrotron works at SOLEIL and at European synchrotron facilities on a range of topics including pigment degradation in paintings, composition of musical instrument varnishes, and provenancing of medieval archaeological ferrous artefacts. Once the platform is fully operational, user support will primarily take place within medium‐term research projects for `hosted' scientists, PhDs and post‐docs. IPANEMA methodological research is focused on advanced two‐dimensional/three‐dimensional imaging and spectroscopy and statistical image analysis, both optimized for ancient materials.     

Radiation damage in soft X-ray microscopy

The rates of chemical transformation by radiation damage of polystyrene (PS), poly(methyl methacrylate) (PMMA), and fibrinogen (Fg) in a X-ray photoemission electron microscope (X-PEEM) and in a scanning transmission X-ray microscope (STXM) have been measured quantitatively using synchrotron radiation. As part of the method of dose evaluation in X-PEEM, the characteristic (1/e) sampling depth of X-PEEM for polystyrene in the C 1s region was measured to be 4 ± 1 nm. Critical doses for chemical change as monitored by changes in the X-ray absorption spectra are 80 (12), 280 (40) and 1230 (180) MGy (1 MGy = 6.242*ρ eV/nm³, where ρ is the polymer density in g/cm³) at 300 eV photon energy for PMMA, Fg and PS, respectively. The critical dose for each material is comparable in X-PEEM and STXM and the values cited are thus the mean of the values determined by X-PEEM and STXM. C 1s, N 1s and O 1s spectroscopy of the damaged materials is used to gain insight into the chemical changes that soft X-rays induce in these materials.     

Energy-filtered XPEEM with NanoESCA using synchrotron and laboratory X-ray sources: Principles and first demonstrated results

The importance of energy filtering in PEEM-based imaging methods has been shown in recent years with the availability of powerful instruments. A new instrument, the NanoESCA, combines a fully electrostatic PEEM column and an aberration corrected double hemispherical analyser as energy filter. This paper reports on recently demonstrated XPEEM results using the first commercially available NanoESCA instrument operated with both synchrotron soft X-rays and monochromatic laboratory Al Kα radiation. The implementation of elemental and bonding-state specific imaging is shown with both excitation sources. The presently achieved (but not yet ultimate) lateral resolutions on energy filtered core-level images are 150 nm with a large synchrotron spot and below 1 μm with a focused laboratory source. To date this is the unique example of laboratory XPEEM core-level imaging.     

Recent applications and current trends in Cultural Heritage Science using synchrotron-based Fourier transform infrared micro-spectroscopy

Synchrotron-based Fourier transform infrared micro-spectroscopy (SR-FTIR) is one of the emerging techniques increasingly employed for Cultural Heritage analytical science. Such a technique combines the assets of FTIR spectroscopy (namely, the identification of molecular groups in various environments: organic/inorganic, crystallized/amorphous, solid/liquid/gas), with the extra potential of chemical imaging (localization of components + easier data treatment thanks to geographical correlations) and the properties of the synchrotron source (namely, high brightness, offering high data quality even with reduced dwell time and reduced spot size).This technique can be applied to nearly all kind of materials found in museum objects, going from hard materials, like metals, to soft materials, like paper, and passing through hybrid materials such as paintings and bones. The purpose is usually the identification of complex compositions in tiny, heterogeneous samples.Recent applications are reviewed in this article, together with the fundamental aspects of the infrared synchrotron source which are leading to such improvements in analytical capabilities. A recent example from the ancient Buddhist paintings from Bamiyan is detailed. Emphasis is made on the true potential offered at such large scale facilities in combining SR-FTIR microscopy with other synchrotron-based micro-imaging techniques. To cite this article: M. Cotte et al., C. R. Physique 10 (2009).     

X-ray and electron microscopy of actinide materials

Actinide materials demonstrate a wide variety of interesting physical properties in both bulk and nanoscale form. To better understand these materials, a broad array of microscopy techniques have been employed, including transmission electron microscopy (TEM), electron energy-loss spectroscopy (EELS), energy dispersive X-ray spectroscopy (EDXS), high-angle annular dark-field imaging (HAADF), scanning electron microscopy (SEM), wavelength dispersive X-ray spectroscopy (WDXS), electron back scattered diffraction (EBSD), scanning tunneling microscopy (STM), atomic force microscopy (AFM), and scanning transmission X-ray microscopy (STXM). Here these techniques will be reviewed, highlighting advances made in the physics, materials science, chemistry, and biology of actinide materials through microscopy. Construction of a spin-polarized TEM will be discussed, considering its potential for examining the nanoscale magnetic structure of actinides as well as broader materials and devices, such as those for computational magnetic memory.     

Using photoelectron emission microscopy with hard-X-rays

We present several successful test cases of using photoelectron emission microscopy (PEEM) for photon energy up to 25 keV. First, the full extended X-ray absorption fine structure analysis was implemented in areas as small as 100 μm² for transition-metal K edge absorption spectra and, therefore, demonstrated the feasibility of combining structural and chemical analysis with hard-X-ray absorption spectroscopy with high lateral resolution. We also show that PEEM can be used in a transmission (radiography) mode as an imaging detector for hard-X-ray. This approach again leads to the unprecedented 0.3 μm lateral resolution, particularly critical for the use of coherence-based phase contrast techniques in real time X-ray radiology.     

The energy dependence of photoelectron peak intensities,Part I: Experimental methods

With the increasing popularity of synchrotron radiation as a tunable photon source for photoemission spectroscopy, the significance of photoelectron peak variation with photon energy is becoming apparent. This variation is due to a number of intrinsic factors (excitation cross section, photon and electron reflection and refraction, inelastic processes, etc.) as well as instrumental factors (monochromator transmission and spectral purity, electron analyzer transmission and resolution, etc.). In this paper we develop methods for factoring out these contributions with the goal of determining the excitation cross section from a peak area measurement. Parts II and III will deal with a range of cross section measurements, and the use of relative peak area information to determine stoichiometry vs. probe depth.     

同步辐射X射线荧光光谱国内外研究进展

同步辐射光源是带电粒子在加速器储存环中以接近光速的速度运动时,沿轨道切线方向发射出的辐射,同步辐射X射线荧光分析(SR-XRF)是以同步辐射X射线作为激发光源的X荧光光谱分析技术.同步辐射X射线荧光分析包括了用于微区及微量元素分析的同步辐射XRF、用于表面及薄膜分析的同步辐射全反射X射线荧光(SR-TXRF)以及用于三...     

同步辐射时间分辨荧光光谱技术

时间分辨光谱技术是研究原子、分子和凝聚态物质的激发动力学，特别是研究发光动力学的有力工具，文章主要介绍以同步辐射为激发光源研究时间分辨光谱的两种方法－时间相关单光子计数法和相移调制法，并比较了两者的优缺点。还讨论了同步辐射光源与其他激发光源相比的特点。     

Microspectroscopic soft X-ray analysis of keratin based biofibers

Scanning soft X-ray transmission microspectroscopy (STXM) and transmission electron microscopy (TEM) have been employed for a high-resolution morphological and chemical analysis of hair fibers from human, sheep and alpaca. STXM allows optimum contrast imaging of the main hair building blocks due to tuneable photon energy. Chemical similarities and deviations for the human hair building blocks as well as for the three investigated species are discussed on the basis of the local near-edge X-ray absorption fine structure (NEXAFS). The spectra of melanosomes corroborate the state-of-the-art model for the chemical structure of eumelanin. Complementary TEM micrographs reveal the occurrence of cortex sectioning in alpaca hair to some extent. A spectroscopic analysis for human hair cortex indicates low mass loss upon soft X-ray irradiation, but transformation of chemical species with decreasing amount of peptide bonds and increasing NEXAFS signal for unsaturated carbon–carbon bonds.     

A scanning transmission X‐ray microscope at the Pohang Light Source

A scanning transmission X‐ray microscope is operational at the 10A beamline at the Pohang Light Source. The 10A beamline provides soft X‐rays in the photon energy range 100–2000 eV using an elliptically polarized undulator. The practically usable photon energy range of the scanning transmission X‐ray microscopy (STXM) setup is from ～150 to ～1600 eV. With a zone plate of 25 nm outermost zone width, the diffraction‐limited space resolution, ～30 nm, is achieved in the photon energy range up to ～850 eV. In transmission mode for thin samples, STXM provides the element, chemical state and magnetic moment specific distributions, based on absorption spectroscopy. A soft X‐ray fluorescence measurement setup has been implemented in order to provide the elemental distribution of thicker samples as well as chemical state information with a space resolution of ～50 nm. A ptychography setup has been implemented in order to improve the space resolution down to 10 nm. Hardware setups and application activities of the STXM are presented.     

VUV synchrotron radiation: a new activation technique for tandem mass spectrometry

A novel experimental technique for tandem mass spectrometry and ion spectroscopy of electrosprayed ions using vacuum‐ultraviolet (VUV) synchrotron radiation is presented. Photon activation of trapped precursor ions has been performed by coupling a commercial linear quadrupole ion trap (Thermo scientific LTQ XL), equipped with the electrosprayed ions source, to the DESIRS beamline at the SOLEIL synchrotron radiation facility. The obtained results include, for the first time on biopolymers, photodetachment spectroscopy using monochromated synchrotron radiation of multi‐charged anions and the single photon ionization of large charge‐selected polycations. The high efficiency and signal‐to‐noise ratio achieved by the present set‐up open up possibilities of using synchrotron light as a new controllable activation method in tandem mass spectrometry of biopolymers and VUV‐photon spectroscopy of large biological ions.     

Trace Analysis of Al on Silicon Surfaces by Ultra‐soft X‐Ray Emission Spectroscopy

It is shown that near normal incidence, low‐energy electron excitation of Al on silicon surfaces by ultra‐soft X‐Ray emission spectroscopy yielded limits of detectibility (LD) in the picogram region. This result on L band emission via electron excitation is fully competitive with photon excitation using K‐α lines via grazing incidence total reflection techniques (TXRF). Surprisingly, it was also found that normal incidence synchrotron photon excitation on the same sample yielded much higher values of LD than low‐energy electron excitation, undoubtedly due to the use of a poor transmission grating used in the entrance optics.     

同步辐射显微技术在高分子材料结构研究中的应用

高分子材料以其优异的性能广泛应用于人类生活的每个角落,但其发展受限于研究手段.基于同步辐射先进光源的研究方法(如散射、吸收和成像等)具有高的空间、时间和能量分辨的优势,是揭示高分子材料多尺度结构形成和演化动力学最有效的工具之一.文章结合作者和国内外同行的工作,以具体案例的形式介绍了同步辐射技术在高分子材料结构研究中的应用.希望能起到抛砖引玉的作用,吸引更多的从事高分子材料结构研究的同行利用同步辐射开展科学研究,同时希望更多的进行物理学研究的同行来帮助回答高分子物理的一些基本科学问题.     

On the interest of synchrotron X-ray imaging for the study of solidification in metallic alloys

Recent developments of more powerful synchrotron sources have led to vast improvements in the performance of X-ray imaging. This is manifested by a continuous increase in the impact of synchrotron experiments in many research areas on materials, in particular solidification science. X-ray imaging has been established as a method of choice for in situ and real-time studies of solidification microstructure formation in metallic alloys, with spatio-temporal resolutions at the scales of relevance. In this article, we present illustrative results of the current capabilities of synchrotron X-ray imaging in this field of research, each of them using different X-ray techniques (radiography, topography and tomography). Those results demonstrate the high potential of these techniques for the investigation of dynamical phenomena in materials processing.     

X射线同轴轮廓成像中影响成像质量的若干因素研究

采用数字模拟方法较为系统地研究了光子能量、样品直径和散射强度对成像质量的影响，克服了已有实验结果的局限性.研究得到成像质量随光子能量的变化关系，模拟结果与已有实验结果相符.研究发现，当其他成像参数不变时，同一样品存在多个光子能量可实现相近的成像质量，且成像质量都较好，这可用于定量相衬成像中多图重构时图像的选择，也为对辐射剂量有要求的样品提供理论依据.得到了不同直径样品在成像质量最佳时所对应的样品到探测器距离，发现这一距离随样品直径的增加而增加.研究了样品厚度或折射率变化导致的散射X射线对成像质量的影响，发 关键词： X射线同轴轮廓成像 成像质量 X射线散射