Lexan coating to eliminate the UV sensitivity of soft x-ray proportional counters with a polypropylene window

Lexan coatings on polypropylene windows can eliminate the UV sensitivity of soft x-ray proportional counters. A method is described for coating thin polypropylene films by dipping into and withdrawing from a volatile solution containing Lexan. The x-ray absorption of a typical Lexan coating was only 7% at 44 A which is small compared to that of 2 microm of polypropylene. The Lexan coatings are stable against vacuum cycling in an environment of UV irradiation. As an external, far-UV filter up to wavelengths of 2400 A, Lexan-coated polypropylene is an interesting alternative to metallic films, particularly when large area, high x-ray transmission, and strength are important.     

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.     

High repetition rate laser produced soft x-ray source for ultrafast x-ray absorption near edge structure measurements

Recent progress in high intensity ultrafast laser systems provides the opportunity to produce laser plasma x-ray sources exhibiting broad spectrum and high average x-ray flux that are well adapted to x-ray absorption measurements. In this paper, the development of a laser based x-ray absorption near edge structure (XANES) beamline exhibiting high repetition rate by using the Advanced Laser Light Source (ALLS) facility 100 Hz laser system (100 mJ, 35 fs at 800 nm) is presented. This system is based on a broadband tantalum solid target soft x-ray source and a grazing incidence grating spectrometer in the 1-5 nm wavelength range. To demonstrate the high potential of this laser based XANES technique in condensed matter physics, material science, or biology, measurements realized with several samples are presented: VO2 vanadium L edge, Si3N4 nitrogen K edge, and BPDA/PPD polyimide carbon K edge. The characteristics of this laser based beamline are discussed in terms of brightness, signal to noise ratio, and compared to conventional synchrotron broadband x-ray sources which allow achieving similar measurements. Apart from the very compact size and the relative low cost, the main advantages of such a laser based soft x-ray source are the picosecond pulse duration and the perfect synchronization between this x-ray probe and a laser pulse excitation which open the way to the realization of time resolved x-ray absorption measurements with picosecond range time resolution to study the dynamics of ultrafast processes and phase transition.     

Fast plasma discharge capillary design as a high power throughput soft x-ray emission source

We present the experimental details and results from a low energy but high repetition rate compact plasma capillary source for extreme ultraviolet and soft x-ray research and applications. Two lengths of capillary are mounted in two versions of a closely related design. The discharge operates in 1.6 and 3.2 mm inner diameter alumina capillaries of lengths 21 and 36 mm. The use of water both as dielectric and as coolant simplifies the compact low inductance design with nanosecond discharge periods. The stored electrical energy of the discharge is approximately 0.5 J and is provided by directly charging the capacitor plates from an inexpensive insulated-gate bipolar transistor in 1?μs or less. We present characteristic argon spectra from plasma between 30 and 300 A? as well as temporally resolved x-ray energy fluence in discrete bands on axis. The spectra also allow the level of ablated wall material to be gauged and associated with useful capillary lifetime according to the chosen configuration and energy storage. The connection between the electron beams associated with the transient hollow cathode mechanism, soft x-ray output, capillary geometry, and capillary lifetime is reported. The role of these e-beams and the plasma as measured on-axis is discussed. The relation of the electron temperature and the ionization stages observed is discussed in the context of some model results of ionization in a non-Maxwellian plasma.     

Characterization of pyrocarbon coated materials using laboratory based x-ray phase contrast imaging technique

In-line x-ray phase contrast is an emerging x-ray imaging technique that promises to improve the contrast in x-ray imaging process. This technique is most suited for x-ray imaging of soft materials, low atomic number elements such as carbon composite fibers, very thin coatings, etc. We have used this new emerging technique for visualization and characterization of the pyrocarbon coated materials using a combination of microfocus x-ray source and x-ray charge coupled device detector. These studies are important for characterization of coating and optimization of various process parameters during deposition. These experiments will help us to exploit the potential of this technique for studies in other areas of material science such as characterization of carbon fibered structures and detection of cracks and flaws in materials. The characterization of the imaging system and optimization of some process parameters for carbon deposition are also described in detail.     

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.     

Equipment for hydrogen absorption-desorption cycling characterization of hydride forming materials

Hydrogen storage materials suffer different degradation processes when they are cycled, forming and decomposing their associated hydride phases. In order to study these processes, we have designed and built an automated apparatus specifically developed for cycling samples of hydride forming materials by changing the external hydrogen pressure. Instead of the standard open configuration involving a high-pressure, high-quality gas bottle and a vacuum pump, the equipment uses another hydride forming material (in our case LaNi5) as a source and sink of hydrogen. The resulting closed-loop configuration eliminates hydrogen waste and ensures that extremely high purity gas is used during the whole experiment, thanks to the purifying properties of the selected hydride as source/sink. Hydrogen pressure is set by changing the source/sink temperature. Cycles can be performed as fast as one cycle every 5 min, a period comparable with typical good hydride forming material kinetics. An example of application of the apparatus is given for 1000 absorption/ desorption cycles on a Mm0.8Ca0.2Ni5 sample.     

Calibration of a high resolution grating soft x-ray spectrometer

The calibration of the soft x-ray spectral response of a large radius of curvature, high resolution grating spectrometer (HRGS) with a back-illuminated charge-coupled device detector is reported. The instrument is cross-calibrated for the 10-50 A? waveband at the Lawrence Livermore National Laboratory electron beam ion trap (EBIT) x-ray source with the EBIT calorimeter spectrometer. The HRGS instrument is designed for laser-produced plasma experiments and is important for making high dynamic range measurements of line intensities, line shapes, and x-ray sources.     

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

The design and performance of a new high-pressure and high-temperature cell for measurement of x-ray absorption fine structure (XAFS) spectra of solid catalysts working in a flowing liquid are presented. The cell has flat, high-purity sintered cubic boron nitride (c-BN) windows which can tolerate high temperature (900 K) and high pressure (10 MPa). The c-BN is a new material which has the highest tensile strength, second only to diamond, and is also chemically and thermally stable. The use of the cell is demonstrated for measurements of PtPdAl(2)O(3) and Ni(2)PSiO(2) hydrodesulfurization catalysts at reaction conditions. A technique called delta chi (Deltachi), involving determining the difference between XAFS spectra of the sample at reaction conditions and the bare sample, is introduced.     

Development of a time-resolved soft x-ray spectrometer for laser produced plasma experiments

A 2400 lines/mm variable-spaced grating spectrometer has been used to measure soft x-ray emission (8-22 A?) from laser-produced plasma experiments at Lawrence Livermore National Laboratory's Compact Multipulse Terrawatt (COMET) Laser Facility. The spectrometer was coupled to a Kentech x-ray streak camera to study the temporal evolution of soft x rays emitted from the back of the Mylar and the copper foils irradiated at 10(15)?W/cm(2). The instrument demonstrated a resolving power of ～120 at 19 A? with a time resolution of 31 ps. The time-resolved copper emission spectrum was consistent with a photodiode monitoring the laser temporal pulse shape and indicated that the soft x-ray emission follows the laser heating of the target. The time and spectral resolutions of this diagnostic make it useful for studies of high temperature plasmas.     

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.     

Note: measurement of the runaway electrons in the J-TEXT tokamak

The runaway electrons have been measured by hard x-ray detectors and soft x-ray array in the J-TEXT tokamak. The hard x-ray radiations in the energy ranges of 0.5-5 MeV are measured by two NaI detectors. The flux of lost runaway electrons can be obtained routinely. The soft x-ray array diagnostics are used to monitor the runaway beam generated in disruptions since the soft x-ray is dominated by the interaction between runaway electrons and metallic impurities inside the plasma. With the aid of soft x-ray array, runaway electron beam has been detected directly during the formation of runaway current plateau following the disruptions.     

Prototype high resolution multienergy soft x-ray array for NSTX

A novel diagnostic design seeks to enhance the capability of multienergy soft x-ray (SXR) detection by using an image intensifier to amplify the signals from a larger set of filtered x-ray profiles. The increased number of profiles and simplified detection system provides a compact diagnostic device for measuring T(e) in addition to contributions from density and impurities. A single-energy prototype system has been implemented on NSTX, comprised of a filtered x-ray pinhole camera, which converts the x-rays to visible light using a CsI:Tl phosphor. SXR profiles have been measured in high performance plasmas at frame rates of up to 10 kHz, and comparisons to the toroidally displaced tangential multi-energy SXR have been made.     

Recent advances in scanning x-ray microscopy

A scanning x-ray microscope has been built at the Daresbury synchrotron radiation source and used to obtain images at soft x-ray wavelengths (～2–4 nm). The focusing element of the microscope is a zone plate, fabricated by a contamination writing process developed at King's College. Zone plates with the finest zone widths, and hence theoretical resolutions, below 20 nm have been fabricated in this way. The contamination material is carbon, and as such is unsuitable for high-efficiency focusing. In order to increase the zone plate efficiency, a shadowing pattern transfer process has been developed and used to replicate contamination lines with 25 nm widths into more suitable materials.     

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.     

In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell

We report a first combination of diamond anvil cell radial x-ray diffraction with in situ laser heating. The laser-heating setup of ALS beamline 12.2.2 was modified to allow one-sided heating of a sample in a diamond anvil cell with an 80 W yttrium lithium fluoride laser while probing the sample with radial x-ray diffraction. The diamond anvil cell is placed with its compressional axis vertical, and perpendicular to the beam. The laser beam is focused onto the sample from the top while the sample is probed with hard x-rays through an x-ray transparent boron-epoxy gasket. The temperature response of preferred orientation of (Fe,Mg)O is probed as a test experiment. Recrystallization was observed above 1500 K, accompanied by a decrease in stress.     

Advanced experimental applications for x-ray transmission gratings spectroscopy using a novel grating fabrication method

A novel fabrication method for soft x-ray transmission grating and other optical elements is presented. The method uses focused-ion-beam technology to fabricate high-quality free standing grating bars on transmission electron microscopy grids. High quality transmission gratings are obtained with superb accuracy and versatility. Using these gratings and back-illuminated CCD camera, absolutely calibrated x-ray spectra can be acquired for soft x-ray source diagnostics in the 100-3000 eV spectral range. Double grating combinations of identical or different parameters are easily fabricated, allowing advanced one-shot application of transmission grating spectroscopy. These applications include spectroscopy with different spectral resolutions, bandwidths, dynamic ranges, and may serve for identification of high-order contribution, and spectral calibrations of various x-ray optical elements.     

Measures for spectral quality in low-voltage X-ray microanalysis

Characteristic x-ray production with energetic electrons depends strongly on the overvoltage, the ratio of the incident beam energy to the critical excitation energy for the atomic species of interest. Low-voltage x-ray microanalysis (beam energy < or = 5 keV) is especially susceptible to artifacts due to sample charging because the overvoltage is low and even slight charging can strongly affect peak intensities. The Duane-Hunt bremsstrahlung limit is a good diagnostic to detect sample charging. Dynamic charging effects, however, can influence spectra despite an apparently satisfactory Duane-Hunt limit. Dynamic charging effects must be examined by time series experiments, or through use of dynamic energy windows continuously measuring count rates placed across the spectrum. When charging is a problem, conductive surface coatings can eliminate the effects. When pristine surfaces must be examined without coating, the use of a conductive grid can control charging so that useful x-ray spectra can be obtained.     

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.