Characterization of the fcc-distorted fcc-structural transition in lanthanum in an extended pressure and temperature range

Abstract

The displacive transition in La is studied in the pressure range up to 26 GPa and under temperatures up to 630 K with angular dispersive X-ray diffraction at the ESRF and with energy dispersive X-ray diffraction in HASYLAB to elucidate further details of this transition with an extension of the transition line up to 22.5(5) GPa and 590(10) K and a determination of the order parameter down to a level of η ≈=5· 10^?4.     

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.     

Soft X-ray microscopy and spectroscopy at the molecular environmental science beamline at the Advanced Light Source

We present examples of the application of synchrotron-based spectroscopies and microscopies to environmentally relevant samples. The experiments were performed at the molecular environmental science beamline (11.0.2) at the Advanced Light Source, Lawrence Berkeley National Laboratory. Examples range from the study of water monolayers on Pt(1 1 1) single crystal surfaces using X-ray emission spectroscopy and the examination of alkali halide solution/water vapor interfaces using ambient pressure photoemission spectroscopy, to the investigation of actinides, river water biofilms, Al-containing colloids and mineral–bacteria suspensions using scanning transmission X-ray spectromicroscopy. The results of our experiments show that spectroscopy and microscopy in the soft X-ray energy range are excellent tools for the investigation of environmentally relevant samples under realistic conditions, i.e., with water or water vapor present at ambient temperature.     

First X-ray fluorescence CT experimental results at the SSRF X-ray imaging beamline

X-ray fluorescence CT is a non-destructive technique for detecting elemental composition and distribution inside a specimen. In this paper, the first experimental results of X-ray fluorescence CT obtained at the SSRF X-ray imaging beamline (BL13W1) are described. The test samples were investigated and the 2D elemental image was reconstructed using a filtered back-projection algorithm. In the sample the element Cd was observed. Up to now, the X-ray fluorescence CT could be carried out at the SSRF X-ray imaging beamline.     

Angular dispersive diffraction using a diamond-anvil pressure cell and synchrotron X-ray source

Abstract

Wavelength dispersive diffraction studies have been performed using a diamond-anvil pressure cell and bending magnet synchrotron produced radiation. A double-crystal monochromator was used to select 15 and 17 keV photons and a 80 μm diameter collimator was used to restrict the beam entering the pressure cavity. Parallelism between the incident beam and the collimator axis was assisted by computer control of the collimator. The image of the transmitted beam was observed using a Hamamatsu x-ray Vidicon and TV monitor, for this alignment. The diffracted beam was recorded on x-ray film using a double film cassette and exposure times ranged from 6 to 8 hours. Neither the exposure time nor the line width of the diffraction lines was significantly altered by replacement of the incident beam collimator with a slit system.     

X射线荧光全息术中消除光源偏振效应和孪生像的重构新算法

以27个铁原子成立方排列的晶体结构为模型,通过数值模拟和重构,讨论了入射光源的偏振性对原子像的影响.结果表明,入射光源的偏振性对原子像的可观测性有非常重要的影响.为此,提出了一种能同时消除光源偏振性影响和全息成像所固有的孪生像的数字重构新算法,并通过数字模拟及重构,结果证明了这是一种有效的数字重构算法,能够解决实验过程中光源偏振性和孪生像对原子像的影响. 关键词： X射线荧光全息术 同步辐射 偏振性     

High pressure structural investigations on hexagonal YInO3

Hexagonal (space group P6₃cm) form of YInO₃ has been investigated under high pressure using synchrotron-based angle-dispersive X-ray diffraction and Raman scattering methods. Our experimental investigations suggest that it undergoes the phase transition to a new phase in the pressure range 12–15?GPa, while the ambient hexagonal phase is found to coexist with the new phase up to 29?GPa. DFT based calculations within the LDA approach on the hexagonal phase of YInO₃ showed that the unit cell volume matches well with the experimentally obtained volume at ambient pressure. As the pressure increases, theoretically obtained values of unit cell volume of the hexagonal phase were found to be significantly lower than that of experimentally obtained values. This discrepancy has been corrected using LDA?+?U_In(4d) (Hubbard interaction parameter between Indium 4d electrons) method. We have proposed the high pressure phase of YInO₃ to be orthorhombic with space group Pnma.     

First X-ray fluorescence CT experimental results at the SSRF X-ray imaging beamline

X-ray fluorescence CT is a non-destructive technique for detecting elemental composition and distribution inside a specimen. In this paper, the first experimental results of X-ray fluorescence CT obtained at the SSRF X-ray imaging beamline (BL13W1) are described. The test samples were investigated and the 2D elemental image was reconstructed using a filtered back-projection algorithm. In the sample the element Cd was observed. Up to now, the X-ray fluorescence CT could be carried out at the SSRF X-ray imaging beamline.     

Polycapillary X-ray lens for the secondary focusing Beijing synchrotron radiation source

According to intensity distribution of the synchrotron radiation source focused by a toroidal mirror at the Beijing synchrotron radiation biological macromolecule station, theoretical modeling of the Beijing synchrotron radiation source is developed for capillary optics. Using this theoretical modeling, the influences of the configuration curve of the polycapillary X-ray lens on transmission efficiency and working distance are analyzed. The experimental results of the transmission efficiency and working distance at the biological macromolecule station are in good agreement with the theoretical results.     

激光同步辐射作为阿秒X射线辐射源的特性研究

 研究了逆流相对论电子与激光脉冲相互作用获得激光同步辐射的频率上移、微分散射截面等特性。发现逆流相对论电子与短脉冲激光相互作用，可以获得阿秒X射线辐射脉冲。短脉冲激光条件下得到的后向散射光的频率上移与长脉冲激光条件下得到的后向散射光的频率上移是完全一致的，同时发现随着入射电子初始能量的增加，散射光的准直性越来越好，后向散射光脉冲的脉宽越来越短。     

An exploration of benchtop X-ray emission spectroscopy for precise characterization of the sulfur redox state in cementitious materials

The evolution of sulfur chemistry in cements is best known in the bailiwick of failure mechanisms via sulfate attack, but is equally important for its contributions to the reduction capacity of cementitious materials often used for immobilizing nuclear waste streams destined for long-term storage, for example, cementitious waste forms (CWF). The total reduction capacity of CWFs, encompassing contributions from both S and Fe reductants, and its implications toward radionuclide immobilization is most often studied by destructive wet chemistry methods requiring acid digestion in the presence of Ce(IV) and subsequent titration and colorimetric interpretation. Here, we investigate a similarly analytical but nondestructive alternative, benchtop high resolution wavelength-dispersive X-ray fluorescence spectroscopy, most commonly known as X-ray emission spectroscopy (XES), for probing the bulk sulfur oxidation state distribution. We present here an initial investigation of S XES, including an improved experimental protocol for lab XES of inhomogeneous samples, both as a complement to the Ce(IV) test and for new scientific opportunities that it enables for observing changes in sulfur chemistry. We discuss future improvements and opportunities, including: (1) the practical challenges associated with coordinating XES and Ce(IV) liquid extraction for a more comprehensive perspective on reduction capacity and for a high-precision evaluation of uncertainties in the Ce(IV) test; and (2) new opportunities, due to the nondestructive nature of XES, for controlled evolution studies aimed at elucidating specific chemical responses of CWFs exposed to invasive gas or liquid species or to accelerated aging by radiative dose or thermal treatment.     

Infrared facility at the Canadian light source

The Canadian Light Source (CLS) is constructing two beamlines for Infrared Spectroscopy using synchrotron radiation (IRSR). One will supply mid-Infrared (2–25 μ) light to a Fourier Transform Infrared (FTIR) spectrometer and microscope for biological applications. The second will have a high resolution FTIR spectrometer for gas-phase and surface spectroscopy in the far-Infrared (beyond 25 μ). The Infrared beamlines will use dipole bending magnet radiation from a special bend magnet port design which provides a 50 mrad square acceptance. Issues with the first mirror and photon mask design, as well as the beamline layout and features are discussed.     

High pressure X-ray diffraction study on BaWO4-II

BaWO₄-II has been synthesized at 5 GPa and 610°C. Its high pressure behavior was studied by in situ synchrotron X-ray diffraction measurements at room temperature up to 17 GPa. BaWO₄-II retains its monoclinic structure. Bulk and axial moduli determined by fitting a third-order Birch–Murnaghan equation of state to lattice parameters are: K ₀=86.2±1.9 GPa, K ₀(a)=56.0±0.9 GPa, K ₀(b)=85.3±2.4 GPa, and K ₀(c)=146.1±3.2 GPa with a fixed K′=4. Analysis of axial compressible modulus shows that the a-axis is 2.61 times more compressible than the c-axis and 1.71 times more compressible than the b-axis. The beta angle decreases smoothly between room pressure and 17 GPa from 93.78° to 90.90°.     

The characterization of Cr secondary oxide phases in ZnO films studied by X-ray spectroscopy and photoemission spectroscopy

X-ray absorption near-edge structure (XANES), X-ray emission spectroscopy (XES), and X-ray photoemission spectroscopy (XPS) were used to characterize the Cr secondary oxide phases in ZnO films that had been prepared using a co-sputtering method. Analysis of the Cr L_3,2-edge XANES spectra reveals that the intensity of white-line features decreases subtly as the sputtering power increases, indicating that the occupation of Cr 3d orbitals increases with Cr concentration in (Zn, Cr)O films. The O K-edge spectra show that the intensity of XANES features of (Zn, Cr)O films is lower than those of ZnO film, suggesting enhanced occupation of O 2p-derived states through O 2p-Cr 3d hybridization. The XES and XPS spectra indicate that the line shapes in the valence band of (Zn, Cr)O films are quite different from those of ZnO and that the Cr₂O₃ phase dominates the spinel structure of (Zn, Cr)O films increasingly as the Cr sputtering power is increased. Over all results suggest that the non-ferromagnetic behavior of (Zn, Cr)O films can be attributed to the dominant presence of Cr₂O₃, whereas the bulk comprise phase segregations of Cr₂O₃ and/or ZnCr₂O₄, which results them the most stable TM-doped ZnO material against etching.     

同步辐射X射线光源在高压科学研究中的应用

同步辐射X射线光源已经成功地应用到高压科学研究的诸多领域.文章简要回顾了同步辐射高压技术的发展历史,简要介绍了同步辐射X射线衍射技术在高压状态方程、强关联体系、地球内部物质以及早期生命起源等研究中的应用.介绍了同步辐射X射线光谱技术(包括晶格振动声子谱的测量)在高压研究中的应用,此外,还介绍了时间分辨的同步辐射技术在冲击压缩研究中的应用,最后展望了未来先进光源应用于高压科学研究的前景.     

A system for doing low temperature-high pressure single crystal X-ray diffraction with a synchrotron source

Abstract

A new diamond anvil cell and a helium flow cryostat have been developed for X-ray diffraction on single crystals at low temperatures and high pressures using white radiation of a synchrotron beam. This novel instrument especially enables continuous change of temperature and pressure of the sample without any adjustment of alignment. Automatic search for diffraction peaks can be performed since less than 30 pm eccentricity can be maintained during the rotation of the cell in the cryostat and the rotation of the cryostat on the goniometer head. The minimum temperature reached is 46 K. Measurements of solid 4He at 11.8 GPa are presented which confirm the stability of the hcp phase on this isobar.     

High-resolution soft X-ray emission spectrograph at advanced light source

The progress of valence electronic spectroscopy with X-rays has been largely limited by the challenge of fine instrumentation. Relatively weak scattering cross-section and/or limited (coarse) energy resolution restrict X-ray spectroscopy to address fundamental issues in condensed-matter electron physics. Depending on the nature of excitations, high brightness photon beam from third-generation synchrotron facilities helps raise the count rates to a detectable limit over the noise level. Over the past decade, it has been realized that high-resolution resonant inelastic soft X-ray scattering has the potential to play an important role in understanding complex phenomena observed in highly correlated systems. Driven by such demand, we have developed a soft X-ray emission spectrograph based on variable line spacing (VLS) gratings to work in the soft X-ray and deep UV (the M edge of transition metals) regime. The slit-less design coupled with high quality optical elements and a high quantum efficiency (QE) in-vacuum CCD detector greatly improves the overall throughput. The M edge spectrograph has been demonstrated to have a resolving power better than 10,000 and will be used in conjunction with meV-resolution beamline (MERLIN) at the Advanced Light Source at Lawrence Berkeley National Laboratory.     

High pressure studies up to 50GPa of CuO

Abstract

Copper oxide has been studied at high pressure up to 50 GPa. A monoclinic structure was compatible with the measurements at all pressures, and no phase change was observed. A bulk modulus, B₀, = 98 GPa, and its pressure derivative B′₀ = 5.6 was obtained.