A highly modular beamline electrostatic levitation facility, optimized for in situ high-energy x-ray scattering studies of equilibrium and supercooled liquids

High-energy x-ray diffraction studies of metallic liquids provide valuable information about structural evolution on the atomic length scale, leading to insights into the origin of the nucleation barrier and the processes of supercooling and glass formation. The containerless processing of the beamline electrostatic levitation (BESL) facility allows coordinated thermophysical and structural studies of equilibrium and supercooled liquids to be made in a contamination-free, high-vacuum (～10(-8) Torr) environment. To date, the incorporation of electrostatic levitation facilities into synchrotron beamlines has been difficult due to the large footprint of the apparatus and the difficulties associated with its transportation and implementation. Here, we describe a modular levitation facility that is optimized for diffraction studies of high-temperature liquids at high-energy synchrotron beamlines. The modular approach used in the apparatus design allows it to be easily transported and quickly setup. Unlike most previous electrostatic levitation facilities, BESL can be operated by a single user instead of a user team.     

Development of a laboratory EXAFS facility

The EXAFS technique is a powerful new structural tool, particularly useful for studies of disordered or otherwise complex materials for which x-ray diffraction techniques are difficult or unfeasible. At the present time, most EXAFS experiments are carried out at a synchrotron facility because of the larger fluxes available. We have developed an in-laboratory apparatus utilizing a focusing crystal technique which increases available fluxes two to three orders of magnitude over previous laboratory facilities, so that EXAFS measurements can be carried out quickly and accurately in the laboratory. We will discuss the principles of the focusing monochromator and we will also illustrate the experimental method with examples, including studies of chemical solutions, defect crystalline solids, and high-temperature superconductors.     

Three-axis acoustic device for levitation of droplets in an open gas stream and its application to examine sulfur dioxide absorption by water droplets

Two acoustic devices to stabilize a droplet in an open gas stream (single-axis and three-axis levitators) have been designed and tested. The gas stream was provided by a jet apparatus with a 64 mm exit diameter and a uniform velocity profile. The acoustic source used was a Langevin vibrator with a concave reflector. The single-axis levitator relied primarily on the radial force from the acoustic field and was shown to be limited because of significant droplet wandering. The three-axis levitator relied on a combination of the axial and radial forces. The three-axis levitator was applied to examine droplet deformation and circulation and to investigate the uptake of SO(2) from the gas stream to the droplet. Droplets ranging in diameters from 2 to 5 mm were levitated in gas streams with velocities up to 9 ms. Droplet wandering was on the order of a half droplet diameter for a 3 mm diameter droplet. Droplet circulation ranged from the predicted Hadamard-Rybczynski pattern to a rotating droplet pattern. Droplet pH over a central volume of the droplet was measured by planar laser induced fluorescence. The results for the decay of droplet pH versus time are in general agreement with published theory and experiments.     

激光等离子体X射线极化光谱研究

为了诊断激光等离子体X射线的极化光谱,研制了一种新型的基于空间分辨的极化谱仪。将平面晶体和球面弯晶色散元件在极化谱仪内正交布置,即在水平通道用PET平面晶体作为色散元件,而在垂直通道用Mica球面弯晶作为色散元件,球面半径为380mm。信号采用成像板进行接收,有效接收面积为30×80mm,从等离子体光源经晶体到成像板的光路约为980mm。物理实验首次在中国工程物理研究院激光聚变研究中心“2×10J激光装置”上进行,成像板获得了铝激光等离子体X射线的光谱空间分辨信号。实验结果表明该谱仪具有较高谱分辨率,适合激光等离子体x射线极化光谱的诊断。     

Electron gun using carbon-nanofiber field emitter

An electron gun constructed using carbon-nanofiber (CNF) emitters and an electrostatic Einzel lens system has been characterized for the development of a high-resolution x-ray source. The CNFs used were grown on tungsten and palladium tips by plasma-enhanced chemical-vapor deposition. Electron beams with the energies of 10相似文献   

Development of an x-ray diffraction camera used in magnetic fields up to 10 T

A high-field x-ray diffraction (HF-XRD) camera was developed to observe structural changes of magnetic materials in magnetic fields up to 10 T. The instrument mainly consists of a Debye-Scherrer-type camera with a diameter of 80.1 mm, a 10-T cryocooled superconducting magnet with a 100-mm room-temperature bore, an x-ray source, a power supply, and a chiller for the x-ray source. An x-ray detector (image plate) in the HF-XRD camera can be taken out and inserted into the magnet without changing the sample position. The performance of the instrument was tested by measuring the HF-XRD for silicon and ferromagnetic MnBi powders. A change of x-ray diffraction pattern was observed due to the magnetic orientation of MnBi, showing that the instrument is useful for studying field-induced orientation processes and structural properties of field-controlled materials.     

Hard x-ray transmission crystal spectrometer at the OMEGA-EP laser facility

The transmission crystal spectrometer (TCS) is approved for taking data at the OMEGA-EP laser facility since 2009 and will be available for the OMEGA target chamber in 2010. TCS utilizes a Cauchois type cylindrically bent transmission crystal geometry with a source to crystal distance of 600 mm. Spectral images are recorded by image plates in four positions, one IP on the Rowland circle and three others at 200, 400, and 600 mm beyond the Rowland circle. An earlier version of TCS was used at LULI on experiments that determined the x-ray source size from spectral line broadening on one IP positioned behind the Rowland circle. TCS has recorded numerous backlighter spectra at EP for point projection radiography and for source size measurements. Hard x-ray source size can be determined from the source broadening of both K shell emission lines and from K absorption edges in the bremsstrahlung continuum, the latter being a new way to measure the spatial extent of the hard x-ray bremsstrahlung continuum.     

Phase-contrast imaging using ultrafast x-rays in laser-shocked materials

High-energy x-rays, >10?keV, can be efficiently produced from ultrafast laser target interactions with many applications to dense target materials in inertial confinement fusion and high-energy density physics. These same x-rays can also be applied to measurements of low-density materials inside high-density Hohlraum environments. In the experiments presented, high-energy x-ray images of laser-shocked polystyrene are produced through phase contrast imaging. The plastic targets are nominally transparent to traditional x-ray absorption but show detailed features in regions of high density gradients due to refractive effects often called phase contrast imaging. The 200 TW Trident laser is used both to produce the x-ray source and to shock the polystyrene target. X-rays at 17 keV produced from 2 ps, 100 J laser interactions with a 12?μm molybdenum wire are used to produce a small source size, required for optimizing refractive effects. Shocks are driven in the 1 mm thick polystyrene target using 2 ns, 250 J, 532 nm laser drive with phase plates. X-ray images of shocks compare well to one-dimensional hydro calculations.     

High energy resolution five-crystal spectrometer for high quality fluorescence and absorption measurements on an x-ray absorption spectroscopy beamline

Fluorescence detection is classically achieved with a solid state detector (SSD) on x-ray absorption spectroscopy (XAS) beamlines. This kind of detection however presents some limitations related to the limited energy resolution and saturation. Crystal analyzer spectrometers (CAS) based on a Johann-type geometry have been developed to overcome these limitations. We have tested and installed such a system on the BM30B/CRG-FAME XAS beamline at the ESRF dedicated to the structural investigation of very dilute systems in environmental, material and biological sciences. The spectrometer has been designed to be a mobile device for easy integration in multi-purpose hard x-ray synchrotron beamlines or even with a laboratory x-ray source. The CAS allows to collect x-ray photons from a large solid angle with five spherically bent crystals. It will cover a large energy range allowing to probe fluorescence lines characteristic of all the elements from Ca (Z = 20) to U (Z = 92). It provides an energy resolution of 1-2 eV. XAS spectroscopy is the main application of this device even if other spectroscopic techniques (RIXS, XES, XRS, etc.) can be also achieved with it. The performances of the CAS are illustrated by two experiments that are difficult or impossible to perform with SSD and the complementarity of the CAS vs SSD detectors is discussed.     

X-ray beam induced current method at the laboratory x-ray source

The x-ray beam induced current method (XBIC) is realized on the laboratory x-ray source using the polycapillary x-ray optics. It is shown that rather good images of grain boundaries in Si can be obtained by this method. The parameters of x-ray beam are estimated by the simulation of Schottky diode image. A good correlation between the experimental and calculated grain boundary XBIC contrast is obtained. The possibilities of laboratory source based XBIC method are estimated.     

A gantry-based tri-modality system for bioluminescence tomography

A gantry-based tri-modality system that combines bioluminescence (BLT), diffuse optical (DOT), and x-ray computed tomography (XCT) into the same setting is presented here. The purpose of this system is to perform bioluminescence tomography using a multi-modality imaging approach. As parts of this hybrid system, XCT and DOT provide anatomical information and background optical property maps. This structural and functional a priori information is used to guide and restrain bioluminescence reconstruction algorithm and ultimately improve the BLT results. The performance of the combined system is evaluated using multi-modality phantoms. In particular, a cylindrical heterogeneous multi-modality phantom that contains regions with higher optical absorption and x-ray attenuation is constructed. We showed that a 1.5 mm diameter bioluminescence inclusion can be localized accurately with the functional a priori information while its source strength can be recovered more accurately using both structural and the functional a priori information.     

A combined small- and wide-angle x-ray scattering detector for measurements on reactive systems

A detector with high dynamic range designed for combined small- and wide-angle x-ray scattering experiments has been developed. It allows measurements on single events and reactive systems, such as particle formation in flames and evaporation of levitating drops. The detector consists of 26 channels covering a region from 0.5° to 60° and it provides continuous monitoring of the sampled signal without readout dead time. The time resolution for fast single events is about 40 μs and for substances undergoing slower dynamics, the time resolution is set to 0.1 or 1 s with hours of continuous sampling. The detector has been used to measure soot particle formation in a flame, burning magnesium and evaporation of a toluene drop in a levitator. The results show that the detector can be used for many different applications with good outcomes and large potential.     

Tunable laboratory extended x-ray absorption fine structure system

A new sensitive x-ray monochromator and detector system for performing extended x-ray absorption fine structure (EXAFS) measurements in the laboratory is described. The monochromator combines x-ray focusing optics with rapid elemental tunability. The detection system effectively removes glitches from the data stream, regardless of whether they are due to impurity lines from the x-ray source or if they are due to random instabilities in the incident beam. Used together with a high intensity rotating anode x-ray source, this system can provide synchrotronlike photon intensities, flexibility and resolution, with the easy access and control possible only in the laboratory.     

Expandable flash x-ray tube (FXT) having a 0.5-mm source size

An inexpensive, expandable, continuously pumped, all-metal flash x-ray tube (FXT) was developed. It was coaxialy integrated at the end of a 70-Omega flexible coaxial transmission line. The tube, which has a small, 0.5-mm, x-ray source size when operated at 200 kV, produces a dose rate of 5x10(7) R/s (at exit port). The produced x-ray pulse has a duration of 20 ns, thus permitting the radiography of high-speed transient phenomena.     

A 9 keV electron-impact liquid-gallium-jet x-ray source

We demonstrate a high-brightness compact 9 keV electron-impact microfocus x-ray source based on a liquid-gallium-jet anode. A approximately 30 W, 50 kV electron gun is focused onto the approximately 20 ms, 30 mum diameter liquid-gallium-jet anode to produce an approximately 10 microm full width at half maximum x-ray spot. The peak spectral brightness is >2 x 10(10) photons(s mm(2) mrad(2)x0.1% BW). Calculation and experiments show potential for increasing this brightness by approximately three orders of magnitude, making the source suitable for laboratory-scale x-ray crystallography and hard x-ray microscopy.     

Compact x-ray microradiograph for in situ imaging of solidification processes: bringing in situ x-ray micro-imaging from the synchrotron to the laboratory

A laboratory based high resolution x-ray radiograph was developed for the investigation of solidification dynamics in alloys. It is based on a low-power microfocus x-ray tube and is potentially appropriate for x-ray diagnostics in space. The x-ray microscope offers a high spatial resolution down to approximately 5 μm. Dynamic processes can be resolved with a frequency of up to 6 Hz. In reference experiments, the setup was optimized to yield a high contrast for AlCu-alloys. With samples of about 150 μm thickness, high quality image sequences of the solidification process were obtained with high resolution in time and space.     

A clamp-type pressure cell for high energy x-ray diffraction

We present a clamp-type pressure cell for high energy x-ray diffraction. The pressure cell was specifically designed for studies of weak superstructure reflections at low temperatures in transition metal oxides, resulting from, e.g., charge density modulations. Using a photon energy of E=100 keV, the bulk properties of single crystals with a volume of typically 2-5 mm3 can be studied in transmission geometry. To demonstrate the performance of the pressure cell, we present data on the charge stripe order in the high-temperature superconductor La1.875Ba0.125CuO4.     

Asymmetric-cut variable-incident-angle monochromator

A novel asymmetric-cut variable-incident-angle monochromator was constructed and tested in 1997 at the Advanced Photon Source of Argonne National Laboratory. The monochromator was originally designed as a high heat load monochromator capable of handling 5-10 kW beams from a wiggler source. This was accomplished by spreading the x-ray beam out on the surface an asymmetric-cut crystal and by using liquid metal cooling of the first crystal. The monochromator turned out to be a highly versatile monochromator that could perform many different types of experiments. The monochromator consisted of two 18° asymmetrically cut Si crystals that could be rotated about 3 independent axes. The first stage (Φ) rotates the crystal around an axis perpendicular to the diffraction plane. This rotation changes the angle of the incident beam with the surface of the crystal without changing the Bragg angle. The second rotation (Ψ) is perpendicular to the first and is used to control the shape of the beam footprint on the crystal. The third rotation (Θ) controls the Bragg angle. Besides the high heat load application, the use of asymmetrically cut crystals allows one to increase or decrease the acceptance angle for crystal diffraction of a monochromatic x-ray beam and allows one to increase or decrease the wavelength bandwidth of the diffraction of a continuum source like a bending-magnet beam or a normal x-ray-tube source. When the monochromator is used in the doubly expanding mode, it is possible to expand the vertical size of the double-diffracted beam by a factor of 10-15. When this was combined with a bending magnet source, it was possible to generate an 8 keV area beam, 16 mm wide by 26 mm high with a uniform intensity and parallel to 1.2 arc sec that could be applied in imaging experiments.     

A new type of x-ray absorption spectrometer

A single-crystal spectrometer for x-ray absorption and emission with a microfocus x-ray source has been set up so that the divergent rays from the source can be analyzed over a wide range of Bragg angles with a high degree of resolution. The covered energy interval depends upon the exposed width of the crystal and the geometrical setup. Preliminary experiments are presented to show the effectiveness of the spectrometer.     

A sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode

A novel sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode based on sample cells with x-ray transparent silicon nitride membranes is introduced. The sample holder allows for a reliable preparation of ultrathin liquid films with an adjustable thickness in the nm-μm range. This enables measurements of high quality x-ray absorption spectra of liquids in transmission mode, as will be shown for the example of liquid H(2)O, aqueous solutions of 3d-transition metal ions and alcohol-water mixtures. The fine structure of the x-ray absorption spectra is not affected by the sample thickness. No effects of the silicon nitride membranes were observed in the spectra. It is shown how an inhomogeneous thickness of the sample affects the spectra and how this can be avoided.