Hard x-ray phase contrast imaging using single absorption grating and hybrid semiconductor pixel detector

A method for x-ray phase contrast imaging is introduced in which only one absorption grating and a microfocus x-ray source in a tabletop setup are used. The method is based on precise subpixel position determination of the x-ray pattern projected by the grating directly from the pattern image. For retrieval of the phase gradient and absorption image (both images obtained from one exposure), it is necessary to measure only one projection of the investigated object. Thus, our method is greatly simplified compared with the phase-stepping method and our method can significantly reduce the time-consuming scanning and possibly the unnecessary dose. Furthermore, the technique works with a fully polychromatic spectrum and gives ample variability in object magnification. Consequently, the approach can open the way to further widespread application of phase contrast imaging, e.g., into clinical practice. The experimental results on a simple testing object as well as on complex biological samples are presented.     

Analyzer-based x-ray phase-contrast microscopy combining channel-cut and asymmetrically cut crystals

An analyzer-based x-ray phase-contrast microscopy (ABM) setup combining a standard analyzer-based x-ray phase-contrast imaging (ABI) setup [nondispersive 4-crystal setup (Bonse-Hart setup)] and diffraction by asymmetrically cut crystals is presented here. An attenuation-contrast microscopy setup with conventional x-ray source and asymmetrically cut crystals is first analyzed. Edge-enhanced effects attributed to phase jumps or refraction/total external reflection on the fiber borders were detected. However, the long exposure times and the possibility to achieve high contrast microscopies by using extremely low attenuation-contrast samples motivated us to assemble the ABM setup using a synchrotron source. This setup was found to be useful for low contrast attenuation samples due to the low exposure time, high contrast, and spatial resolution found. Moreover, thanks to the combination with the nondispersive ABI setup, the diffraction-enhanced x-ray imaging algorithm could be applied.     

Inspection of refractive X-ray lenses using high-resolution differential phase contrast imaging with a microfocus X-ray source

A refractive x-ray lens was characterized using a magnifying cone beam setup for differential phase contrast imaging in combination with a microfocus x-ray tube. Thereby, the differential and the total phase shift of x rays transmitted through the lens were determined. Lens aberrations have been characterized based on these refractive properties.     

硬X射线相衬成像及其生物应用

X射线相衬技术大大拓宽X射线的应用领域。本文综述X射线相衬成像的物理学原理、X射线相衬成像装置的一般结构和应用方法,并对各种不同相衬成像的方法、成像算法和生物应用逐一阐述。     

X-ray grating interferometer for materials-science imaging at a low-coherent wiggler source

X-ray phase-contrast radiography and tomography enable to increase contrast for weakly absorbing materials. Recently, x-ray grating interferometers were developed that extend the possibility of phase-contrast imaging from highly brilliant radiation sources like third-generation synchrotron sources to non-coherent conventional x-ray tube sources. Here, we present the first installation of a three grating x-ray interferometer at a low-coherence wiggler source at the beamline W2 (HARWI II) operated by the Helmholtz-Zentrum Geesthacht at the second-generation synchrotron storage ring DORIS (DESY, Hamburg, Germany). Using this type of the wiggler insertion device with a millimeter-sized source allows monochromatic phase-contrast imaging of centimeter sized objects with high photon flux. Thus, biological and materials-science imaging applications can highly profit from this imaging modality. The specially designed grating interferometer currently works in the photon energy range from 22 to 30 keV, and the range will be increased by using adapted x-ray optical gratings. Our results of an energy-dependent visibility measurement in comparison to corresponding simulations demonstrate the performance of the new setup.     

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.     

Time-resolved soft x-ray absorption setup using multi-bunch operation modes at synchrotrons

Here, we report on a novel experimental apparatus for performing time-resolved soft x-ray absorption spectroscopy in the sub-ns time scale using non-hybrid multi-bunch mode synchrotron radiation. The present setup is based on a variable repetition rate Ti:sapphire laser (pump pulse) synchronized with the ~500 MHz x-ray synchrotron radiation bunches and on a detection system that discriminates and singles out the significant x-ray photon pulses by means of a custom made photon counting unit. The whole setup has been validated by measuring the time evolution of the L(3) absorption edge during the melting and the solidification of a Ge single crystal irradiated by an intense ultrafast laser pulse. These results pave the way for performing synchrotron time-resolved experiments in the sub-ns time domain with variable repetition rate exploiting the full flux of the synchrotron radiation.     

Quantitative studies on inner interfaces in conical metal joints using hard x-ray inline phase contrast radiography

Quantitative investigation of micrometer and submicrometer gaps between joining metal surfaces is applied to conical plug-socket connections in dental titanium implants. Microgaps of widths well beyond the resolving power of industrial x-ray systems are imaged by synchrotron phase contrast radiography. Furthermore, by using an analytical model for the relatively simple sample geometry and applying it to numerical forward simulations of the optical Fresnel propagation, we show that quantitative measurements of the microgap width down to 0.1?μm are possible. Image data recorded at the BAMline (BESSY-II light source, Germany) are presented, with the resolving power of the imaging system being 4?μm in absorption mode and ～14?μm in phase contrast mode (z(2)=0.74?m). Thus, phase contrast radiography, combined with numerical forward simulations, is capable of measuring the widths of gaps that are two orders of magnitude thinner than the conventional detection limit.     

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.     

Development of optics for x-ray phase-contrast imaging of high energy density plasmas

Phase-contrast or refraction-enhanced x-ray radiography can be useful for the diagnostic of low-Z high energy density plasmas, such as imploding inertial confinement fusion (ICF) pellets, due to its sensitivity to density gradients. To separate and quantify the absorption and refraction contributions to x-ray images, methods based on microperiodic optics, such as shearing interferometry, can be used. To enable applying such methods with the energetic x rays needed for ICF radiography, we investigate a new type of optics consisting of grazing incidence microperiodic mirrors. Using such mirrors, efficient phase-contrast imaging systems could be built for energies up to ～100?keV. In addition, a simple lithographic method is proposed for the production of the microperiodic x-ray mirrors based on the difference in the total reflection between a low-Z substrate and a high-Z film. Prototype mirrors fabricated with this method show promising characteristics in laboratory tests.     

Intercomparison of gamma scattering, gammatography, and radiography techniques for mild steel nonuniform corrosion detection

This paper focuses on the mild steel (MS) corrosion detection and intercomparison of results obtained by gamma scattering, gammatography, and radiography techniques. The gamma scattering non-destructive evaluation (NDE) method utilizes scattered gamma radiation for the detection of corrosion, and the scattering experimental setup is an indigenously designed automated personal computer (PC) controlled scanning system consisting of computerized numerical control (CNC) controlled six-axis source detector system and four-axis job positioning system. The system has been successfully used to quantify the magnitude of corrosion and the thickness profile of a MS plate with nonuniform corrosion, and the results are correlated with those obtained from the conventional gammatography and radiography imaging measurements. A simple and straightforward reconstruction algorithm to reconstruct the densities of the objects under investigation and an unambiguous interpretation of the signal as a function of material density at any point of the thick object being inspected is described. In this simple and straightforward method the density of the target need not be known and only the knowledge of the target material's mass attenuation coefficients (composition) for the incident and scattered energies is enough to reconstruct the density of the each voxel of the specimen being studied. The Monte Carlo (MC) numerical simulation of the phenomena is done using the Monte Carlo N-Particle Transport Code (MCNP) and the quantitative estimates of the values of signal-to-noise ratio for different percentages of MS corrosion derived from these simulations are presented and the spectra are compared with the experimental data. The gammatography experiments are carried out using the same PC controlled scanning system in a narrow beam, good geometry setup, and the thickness loss is estimated from the measured transmitted intensity. Radiography of the MS plates is carried out using 160 kV x-ray machine. The digitized radiographs with a resolution of 50 μm are processed for the detection of corrosion damage in five different locations. The thickness losses due to the corrosion of the MS plate obtained by gamma scattering method are compared with those values obtained by gammatography and radiography techniques. The percentage thickness loss estimated at different positions of the corroded MS plate varies from 17.78 to 27.0, from 18.9 to 24.28, and from 18.9 to 24.28 by gamma scattering, gammatography, and radiography techniques, respectively. Overall, these results are consistent and in line with each other.     

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.     

Differential phase contrast x-ray microimaging with scanning-imaging x-ray microscope optics

A novel x-ray microimaging system that consists of a scanning microscope optics with a one-dimensional focusing (line-focusing) device and an imaging microscope optics with a one-dimensional objective is developed. These two optical systems are set normal to each other regarding the optical axis. A two-dimensional image is obtained with one-dimensional translation scan of the line probe. During scans, positional data in the normal to the scanning direction are obtained simultaneously with the imaging microscope optics. Differential phase contrast (DPC) image and absorption contrast (AC) image can be arbitrarily obtained by image processing after data acquisition. Preliminary experiment has been carried out by using a couple of one-dimensional Fresnel zone plate as the linear-focusing device and the one-dimensional objective. Two-dimensional DPC and AC images of test sample have been successfully obtained with 8 keV x-rays.     

Dual-plane ultrafast limited-angle electron beam x-ray tomography

Electron beam x-ray tomography is an imaging technique, which can provide cross-sectional images of an object of interest with about 1 mm spatial resolution at frame rates of up to 10,000 frames per second. As a non-intrusive method it is especially suited for studying multiphase flows. For this purpose we devised an experimental limited-angle scan setup which utilizes linear beam deflection to generate radiographic projections. This setup was employed in the study of gas–liquid flow in an experimental flow loop operated at different liquid and gas flow rates. Electron-beam tomography images were compared with image data of a wire-mesh sensor. The latter is a fast but intrusive imaging device which is commonly used in gas–liquid flow imaging and achieves comparable frame rates but at lower spatial resolution. As a novelty we implemented a dual-plane limited-angle electron beam x-ray tomography which allows us to gain information about the phase velocities using cross-correlation data analysis.     

Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime

The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam.     

Evaluation of rapid volume changes of substrate-adherent cells by conventional microscopy 3D imaging

Precise measurement of rapid volume changes of substrate‐adherent cells is essential to understand many aspects of cell physiology, yet techniques to evaluate volume changes with sufficient precision and high temporal resolution are limited. Here, we describe a novel imaging method that surveys the rapid morphology modifications of living, substrate‐adherent cells based on phase‐contrast, digital video microscopy. Cells grown on a glass substrate are mounted in a custom‐designed, side‐viewing chamber and subjected to hypotonic swelling. Side‐view images of the rapidly swelling cell, and at the end of the assay, an image of the same cell viewed from a perpendicular direction through the substrate, are acquired. Based on these images, off‐line reconstruction of 3D cell morphology is performed, which precisely measures cell volume, height and surface at different points during cell volume changes. Volume evaluations are comparable to those obtained by confocal laser scanning microscopy (ΔVolume ≤ 14%), but our method has superior temporal resolution limited only by the time of single‐image acquisition, typically ～100 ms. The advantages of using standard phase‐contrast microscopy without the need for cell staining or intense illumination to monitor cell volume make this system a promising new tool to investigate the fundamentals of cell volume physiology.     

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.     

A combined ion-sputtering and electron-beam annealing device for the in vacuo postpreparation of scanning probes

We describe the setup, characteristics, and application of an in vacuo ion-sputtering and electron-beam annealing device for the postpreparation of scanning probes (e.g., scanning tunneling microscopy (STM) tips) under ultrahigh vacuum (UHV) conditions. The proposed device facilitates the straightforward implementation of a common two-step cleaning procedure, where the first step consists of ion-sputtering, while the second step heals out sputtering-induced defects by thermal annealing. In contrast to the standard way, no dedicated external ion-sputtering gun is required with the proposed device. The performance of the described device is demonstrated by SEM micrographs and energy dispersive x-ray characterization of electrochemically etched tungsten tips prior and after postprocessing.     

Time-resolved near-edge x-ray absorption fine structure spectroscopy on photo-induced phase transitions using a tabletop soft-x-ray spectrometer

We present a table-top soft-x-ray spectrometer for the wavelength range λ = 1-5 nm based on a stable laser-driven x-ray source, making use of a gas-puff target. With this setup, optical light-pump/soft-x-ray probe near-edge x-ray absorption fine structure (NEXAFS) experiments with a temporal resolution of about 230 ps are feasible. Pump-probe NEXAFS measurements were carried out in the "water-window" region (2.28 nm-4.36 nm) on the manganite Pr(0.7)Ca(0.3)MnO(3), investigating diminutive changes of the oxygen K edge that derive from an optically induced phase transition. The results show the practicability of the table-top soft-x-ray spectrometer on demanding investigations so far exclusively conducted at synchrotron radiation sources.     

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (～2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.