Simultaneous surface plasmon resonance and x-ray absorption spectroscopy

We present an experimental setup for the simultaneous measurement of surface plasmon resonance (SPR) and x-ray absorption spectroscopy (XAS) on metallic thin films at a synchrotron beamline. The system allows measuring in situ and in real time the effect of x-ray irradiation on the SPR curves to explore the interaction of x-rays with matter. It is also possible to record XAS spectra while exciting SPR in order to study changes in the films induced by the excitation of surface plasmons. Combined experiments recording simultaneously SPR and XAS curves while scanning different parameters can be also carried out. The relative variations in the SPR and XAS spectra that can be detected with this setup range from 10(-3) to 10(-5), depending on the particular experiment.     

Transmissive x-ray beam position monitors with submicron position- and submillisecond time resolution

We present the development of fast transmissive center-of-mass x-ray beam position monitors with a large active area, based on a thinned position sensitive detector in both a duo- and a tetra-lateral variant. The detectors were tested at BESSY beamlines BL14.1, KMC-1, and KMC-2 and yielded signal currents of up to 3 microA/100 mA ring current at 10 keV photon energy using the monochromatic focused beam of BL14.1. The active area sizes were 1 x 1 and 3 x 3 mm(2) for the duo-lateral and 5 x 5 mm(2) for the tetra-lateral devices, with the duo-lateral detectors currently being available in sizes from 1 x 1 to 10 x 10 mm(2) and thicknesses between 5 and 10 microm. The presented detectors' thicknesses were measured to be 5 and 8 microm with a corresponding transmission of up to 93% at 10 keV and 15% at 2.5 keV. Up to a detection bandwidth of 10 kHz, the monitors provide submicron position resolution. For lower detection bandwidths, the signal-to-noise reaches values of up to 6 x 10(4) at 10 Hz, corresponding to a position resolution of better than 50 nm for both detector sizes. As it stands, this monitor design approach promises to be a generic solution for automation of state-of-the-art crystal monochromator beamlines.     

High-performance soft x-ray spectromicroscopy beamline at SSRF

The Shanghai Synchrotron Radiation Facility (SSRF) is the first third-generation synchrotron facility in China and operated at an electron energy of 3.5 GeV. One of the seven beamlines in the first construction phase is devoted to soft x-ray spectromicroscopy and is equipped with an elliptically polarized undulator light source, a plane grating monochromator, and a scanning transmission x-ray microscope end station. Initial results reveal the high performance of this beamline, with an energy resolving power estimated to be over 10,000 at the argon L-edge and a spatial resolution better than 30 nm.     

Confocal micro-x-ray fluorescence spectrometer for light element analysis

An existing micro-x-ray fluorescence (micro-XRF) spectrometer designed for light element analysis (6 ≤ Z ≤ 14) has been extended to confocal geometry: a second polycapillary x-ray optic has been introduced in front of the energy dispersive x-ray detector. New piezo positioners for optimum alignment of both optics have been installed inside the vacuum chamber. The spectrometer offers now the possibility of true 3D elemental analysis in the micrometer regime. Depth resolution varies between 100 μm at 1 keV fluorescence energy (Na-Kα) and 30 μm for 17.5 keV (Mo). To further extend analytical capabilities a second x-ray tube with a Rh anode has been acquired to supplement to existing Mo anode tube. Lower limits of detection have been determined to be in the ppm region for confocal geometry. The spectrometer has been characterized and tested using different samples. Furthermore, results have been compared with SR micro-XRF to show the capabilities and limitations of this spectrometer.     

Continuous flow time-resolved small-angle x-ray scattering and X-ray absorption spectroscopy

A continuous flow device to characterize the growth of nanometer particles was assembled. In-situ millisecond or second-order time-resolved small angle x-ray scattering and x-ray absorption spectroscopy was performed using this device at the Beijing Synchrotron Radiation Facility. The time resolution was adjusted from 10 ms to 1.0 s by changing the flow rate of the solution. The temperature was variable from 5–95°C. Custom-designed pulse eliminators were employed to eliminate adverse pump fluctuations and improve the quality of measurements. The system was used to characterize zinc sulfide nanoparticles by small angle x-ray scattering and x-ray absorption spectroscopy.     

X-ray excited optical luminescence detection by scanning near-field optical microscope: a new tool for nanoscience

Investigations of complex nanostructured materials used in modern technologies require special experimental techniques able to provide information on the structure and electronic properties of materials with a spatial resolution down to the nanometer scale. We tried to address these needs through the combination of x-ray absorption spectroscopy (XAS) using synchrotron radiation microbeams with scanning near-field optical microscopy (SNOM) detection of the x-ray excited optical luminescence (XEOL) signal. This new instrumentation offers the possibility to carry out a selective structural analysis of the sample surface with the subwavelength spatial resolution determined by the SNOM probe aperture. In addition, the apex of the optical fiber plays the role of a topographic probe, and chemical and topographic mappings can be simultaneously recorded. Our working XAS-SNOM prototype is based on a quartz tuning-fork head mounted on a high stability nanopositioning system; a coated optical fiber tip, operating as a probe in shear-force mode; a detection system coupled with the microscope head control system; and a dedicated software/hardware setup for synchronization of the XEOL signal detection with the synchrotron beamline acquisition system. We illustrate the possibility to obtain an element-specific contrast and to perform nano-XAS experiments by detecting the Zn K and W L(3) absorption edges in luminescent ZnO and mixed ZnWO(4)-ZnO nanostructured thin films.     

Design and performance of a versatile curved-crystal spectrometer for high-resolution spectroscopy in the tender x-ray range

A complete in-vacuum curved-crystal x-ray emission spectrometer in Johansson geometry has been constructed for a 2-6 keV energy range with sub natural line-width energy resolution. The spectrometer is designed to measure x-ray emission induced by photon and charged particle impact on solid and gaseous targets. It works with a relatively large x-ray source placed inside the Rowland circle and employs position sensitive detection of diffracted x-rays. Its compact modular design enables fast and easy installation at a synchrotron or particle accelerator beamline. The paper presents main characteristics of the spectrometer and illustrates its capabilities by showing few selected experimental examples.     

A tabletop femtosecond time-resolved soft x-ray transient absorption spectrometer

A laser-based, tabletop instrument is constructed to perform femtosecond soft x-ray transient absorption spectroscopy. Ultrashort soft x-ray pulses produced via high-order harmonic generation of the amplified output of a femtosecond Ti:sapphire laser system are used to probe atomic core-level transient absorptions in atoms and molecules. The results provide chemically specific, time-resolved dynamics with sub-50-fs time resolution. In this setup, high-order harmonics generated in a Ne-filled capillary waveguide are refocused by a gold-coated toroidal mirror into the sample gas cell, where the soft x-ray light intersects with an optical pump pulse. The transmitted high-order harmonics are spectrally dispersed with a homebuilt soft x-ray spectrometer, which consists of a gold-coated toroidal mirror, a uniform-line spaced plane grating, and a soft x-ray charge coupled device camera. The optical layout of the instrument, design of the soft x-ray spectrometer, and spatial and temporal characterizations of the high-order harmonics are described. Examples of static and time-resolved photoabsorption spectra collected on this apparatus are presented.     

Relative detection efficiency of back- and front-illuminated charge-coupled device cameras for X-rays between 1 keV and 18 keV

High-resolution x-ray measurements were performed with a von Hamos-type bent crystal spectrometer using for the detection of the diffracted photons either a back-illuminated charge-coupled device (CCD) camera or a front-illuminated one. For each CCD the main x-ray emission lines (e.g., Kalpha, Kbeta, Lalpha, and Lbeta) of a variety of elements were measured in order to probe the performances of the two detectors between 1 and 18 keV. From the observed x-ray lines the linearity of the energy response, the noise level, the energy resolution, and the quantum efficiency ratio of the two CCDs were determined.     

A high resolution and large solid angle x-ray Raman spectroscopy end-station at the Stanford Synchrotron Radiation Lightsource

We present a new x-ray Raman spectroscopy end-station recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The end-station is located at wiggler beamline 6-2 equipped with two monochromators-Si(111) and Si(311) as well as collimating and focusing optics. It consists of two multi-crystal Johann type spectrometers arranged on intersecting Rowland circles of 1 m diameter. The first one, positioned at the forward scattering angles (low-q), consists of 40 spherically bent and diced Si(110) crystals with 100 mm diameters providing about 1.9% of 4π sr solid angle of detection. When operated in the (440) order in combination with the Si (311) monochromator, an overall energy resolution of 270 meV is obtained at 6462.20 eV. The second spectrometer, consisting of 14 spherically bent Si(110) crystal analyzers (not diced), is positioned at the backward scattering angles (high-q) enabling the study of non-dipole transitions. The solid angle of this spectrometer is about 0.9% of 4π sr, with a combined energy resolution of 600 meV using the Si (311) monochromator. These features exceed the specifications of currently existing relevant instrumentation, opening new opportunities for the routine application of this photon-in/photon-out hard x-ray technique to emerging research in multidisciplinary scientific fields, such as energy-related sciences, material sciences, physical chemistry, etc.     

A synchrotron beamline for delivering high purity vacuum ultraviolet photons

We report on the current status and performance of the toroidal grating monochromator beamline at the Brazilian Synchrotron Light Laboratory (Laboratorio Nacional de Luz Sincrotron). This beamline provides photons in the vacuum ultraviolet and soft x-ray regions from 12 to 330 eV with three interchangeable gratings. We report on the improvement, which allows the possibility of choosing the light polarization degree from linear to almost circular. Here, we also describe the development of a new apparatus, namely, the mirror-inserted harmonic attenuator and calibrating-device with a long length (MIRHACLLE). All beamlines based on diffraction gratings suffer from the problem of high harmonics contaminations to some extent. The MIRHACLLE provides a way to efficiently suppress high harmonics from 25% to 1 ppm in a grazing incidence bending magnet beamline. Its principle of operation relays on the absorption of the high energy photons in a gas phase region. It allows negligible high harmonics contamination for photon energies ranging from 12 eV to the gas first ionization threshold, 21.6 eV, in the case of neon. We also demonstrate the possibility to use this device for energy calibration and resolution evaluation together with any experiment needing its filtering capabilities. The device is also very cost effective compared to other filters presented previously in the literature.     

Core-hole effects on energy-loss near-edge structure

We present first-principles electron energy-loss near-edge structure calculations that incorporate electron-hole interactions and are in excellent agreement with experimental data obtained with X-ray absorption spectroscopy (XAS) and electron energy-loss spectroscopy (EELS). The superior energy resolution in XAS spectra and the new calculations make a compelling case that core-hole effects dominate core-excitation edges of the materials investigated: Si, SiO2, MgO, and SiC. These materials differ widely in the dielectric constant leading to the conclusion that core-hole effects dominate all core-electron excitation spectra in semiconductors and insulators. The implications of the importance of core-holes for simulations of core-electron excitation spectra at interfaces will be discussed.     

A high-repetition rate scheme for synchrotron-based picosecond laser pump/x-ray probe experiments on chemical and biological systems in solution

We present the extension of time-resolved optical pump/x-ray absorption spectroscopy (XAS) probe experiments towards data collection at MHz repetition rates. The use of a high-power picosecond laser operating at an integer fraction of the repetition rate of the storage ring allows exploitation of up to two orders of magnitude more x-ray photons than in previous schemes based on the use of kHz lasers. Consequently, we demonstrate an order of magnitude increase in the signal-to-noise of time-resolved XAS of molecular systems in solution. This makes it possible to investigate highly dilute samples at concentrations approaching physiological conditions for biological systems. The simplicity and compactness of the scheme allows for straightforward implementation at any synchrotron beamline and for a wide range of x-ray probe techniques, such as time-resolved diffraction or x-ray emission studies.     

Note: study of extreme ultraviolet and soft x-ray emission of metal targets produced by laser-plasma-interaction

Different metal targets were investigated as possible source material for tailored laser-produced plasma-sources. In the wavelength range from 1 to 20 nm, x-ray spectra were collected with a calibrated spectrometer with a resolution of λ/Δλ = 150 at 1 nm up to λ/Δλ = 1100 at 15 nm. Intense line emission features of highly ionized species as well as continuum-like spectra from unresolved transitions are presented. With this knowledge, the optimal target material can be identified for the envisioned application of the source in x-ray spectrometry on the high energy side of the spectra at about 1 keV. This energy is aimed for because 1 keV-radiation is ideally suited for L-shell x-ray spectroscopy with nm-depth resolution.     

An upgraded x-ray spectroscopy diagnostic on MST

An upgraded x-ray spectroscopy diagnostic is used to measure the distribution of fast electrons in MST and to determine Z(eff) and the particle diffusion coefficient D(r). A radial array of 12 CdZnTe hard-x-ray detectors measures 10-150 keV Bremsstrahlung from fast electrons, a signature of reduced stochasticity and improved confinement in the plasma. A new Si soft-x-ray detector measures 2-10 keV Bremsstrahlung from thermal and fast electrons. The shaped output pulses from both detector types are digitized and the resulting waveforms are fit with Gaussians to resolve pileup and provide good time and energy resolution. Lead apertures prevent detector saturation and provide a well-known etendue, while lead shielding prevents pickup from stray x-rays. New Be vacuum windows transmit >2?keV x-rays, and additional Al and Be filters are sometimes used to reduce low energy flux for better resolution at higher energies. Measured spectra are compared to those predicted by the Fokker-Planck code CQL3D to deduce Z(eff) and D(r).     

A multi-crystal wavelength dispersive x-ray spectrometer

A multi-crystal wavelength dispersive hard x-ray spectrometer with high-energy resolution and large solid angle collection is described. The instrument is specifically designed for time-resolved applications of x-ray emission spectroscopy (XES) and x-ray Raman scattering (XRS) at X-ray Free Electron Lasers (XFEL) and synchrotron radiation facilities. It also simplifies resonant inelastic x-ray scattering (RIXS) studies of the whole 2d RIXS plane. The spectrometer is based on the Von Hamos geometry. This dispersive setup enables an XES or XRS spectrum to be measured in a single-shot mode, overcoming the scanning needs of the Rowland circle spectrometers. In conjunction with the XFEL temporal profile and high-flux, it is a powerful tool for studying the dynamics of time-dependent systems. Photo-induced processes and fast catalytic reaction kinetics, ranging from femtoseconds to milliseconds, will be resolvable in a wide array of systems circumventing radiation damage.     

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.     

KMC-1: a high resolution and high flux soft x-ray beamline at BESSY

The crystal monochromator beamline KMC-1 at a BESSY II bending magnet covers the energy range from soft (1.7 keV) to hard x-rays (12 keV) employing the (n,-n) double crystal arrangement with constant beam offset. The monochromator is equipped with three sets of crystals, InSb, Si (111), and Si (422) which are exchangeable in situ within a few minutes. Beamline and monochromator have been optimized for high flux and high resolution. This could be achieved by (1) a windowless setup under ultrahigh-vacuum conditions up to the experiment, (2) by the use of only three optical elements to minimize reflection losses, (3) by collecting an unusually large horizontal radiation fan (6 mrad) with the toroidal premirror, and (4) the optimization of the crystal optics to the soft x-ray range necessitating quasibackscattering crystal geometry (theta(Bragg,max)=82 degrees) delivering crystal limited resolution. The multipurpose beamline is in use for a variety of user facilities such as extended x-ray absorption fine structure, ((Bio-)EXAFS) near-edge x-ray absorption fine structure (NEXAFS), absorption and fluorescence spectroscopy. Due to the windowless UHV setup the k edges of the technologically and biologically important elements such as Si, P, and S are accessible. In addition to these experiments this beamline is now extensively used for photoelectron spectroscopy at high kinetic energies. Photon flux in the 10(11)-10(12) photons/s range and beamline resolving powers of more than E/DeltaE approximately 100.000 have been measured at selected energies employing Si (nnn) high order radiation in quasibackscattering geometry, thus photoelectron spectroscopy with a total instrumental resolution of about 150 meV is possible. This article describes the design features of the beamline and reports some experimental results in the above mentioned fields.     

High resolution absorption spectroscopy of exploding wire plasmas using an x-pinch x-ray source and spherically bent crystal

We present here the use of absorption spectroscopy of the continuum radiation from x-pinch-produced point x-ray sources as a diagnostic to investigate the properties of aluminum plasmas created by pulsed power machines. This technique is being developed to determine the charge state, temperature, and density as a function of time and space under conditions that are inaccessible to x-ray emission spectroscopic diagnostics. The apparatus and its characterization are described, and the spectrometer dispersion, magnification, and resolution are calculated and compared with experimental results. Spectral resolution of about 5000 and spatial resolution of about 20 μm are demonstrated. This spectral resolution is the highest available to date in an absorption experiment. The beneficial properties of the x-pinch x-ray source as the backlighter for this diagnostic are the small source size (<5 μm), smooth continuum radiation, and short pulse duration (<0.1 ns). Results from a closely spaced (1 mm) exploding wire pair are shown and the general features are discussed.     

Linear position-sensitive x-ray detector incorporating a self-scanning photodiode array

A linear position-sensitive x-ray detector for x-ray spectroscopy and diffraction applications has been tested which can provide excellent spatial resolution, wide dynamic range and good sensitivity. The heart of the system is a self-scanning, photosensitive silicon diode array. It is interfaced via fiber optics to a thin layer of ZnS which fluoresces visible light upon absorption of x-radiation. The conversion to visible light and optical coupling provide several-fold gain in the efficiency of detection as compared to the direct detection of x-ray by the diode array. Equally important is that the array is protected from irreversible damage by high energy radiation, a limitation which previously hindered this application of silicon diode technology.