Performance analysis of quantitative phase retrieval method in Zernike phase contrast X-ray microscopy

Since the invention of Zernike phase contrast method in 1930,it has been widely used in optical microscopy and more recently in X-ray microscopy.Considering the image contrast is a mixture of absorption and phase information,we recently have proposed and demonstrated a method for quantitative phase retrieval in Zernike phase contrast X-ray microscopy.In this contribution,we analyze the performance of this method at different photon energies.Intensity images of PMMA samples are simulated at 2.5 keV and 6.2 keV,respectively,and phase retrieval is performed using the proposed method.The results demonstrate that the proposed phase retrieval method is applicable over a wide energy range.For weakly absorbing features,the optimal photon energy is 2.5 keV,from the point of view of image contrast and accuracy of phase retrieval.On the other hand,in the case of strong absorption objects,a higher photon energy is preferred to reduce the error of phase retrieval.These results can be used as guidelines to perform quantitative phase retrieval in Zernike phase contrast X-ray microscopy with the proposed method.     

Characterization of an in‐vacuum PILATUS 1M detector

A dedicated in‐vacuum X‐ray detector based on the hybrid pixel PILATUS 1M detector has been installed at the four‐crystal monochromator beamline of the PTB at the electron storage ring BESSY II in Berlin, Germany. Owing to its windowless operation, the detector can be used in the entire photon energy range of the beamline from 10 keV down to 1.75 keV for small‐angle X‐ray scattering (SAXS) experiments and anomalous SAXS at absorption edges of light elements. The radiometric and geometric properties of the detector such as quantum efficiency, pixel pitch and module alignment have been determined with low uncertainties. The first grazing‐incidence SAXS results demonstrate the superior resolution in momentum transfer achievable at low photon energies.     

Towards tender X‐rays with Zernike phase‐contrast imaging of biological samples at 50 nm resolution

X‐ray microscopy is a commonly used method especially in material science application, where the large penetration depth of X‐rays is necessary for three‐dimensional structural studies of thick specimens with high‐Z elements. In this paper it is shown that full‐field X‐ray microscopy at 6.2 keV can be utilized for imaging of biological specimens with high resolution. A full‐field Zernike phase‐contrast microscope based on diffractive optics is used to study lipid droplet formation in hepatoma cells. It is shown that the contrast of the images is comparable with that of electron microscopy, and even better contrast at tender X‐ray energies between 2.5 keV and 4 keV is expected.     

Characterization of a quadrant diamond transmission X‐ray detector including a precise determination of the mean electron–hole pair creation energy

Precise monitoring of the incoming photon flux is crucial for many experiments using synchrotron radiation. For photon energies above a few keV, thin semiconductor photodiodes can be operated in transmission for this purpose. Diamond is a particularly attractive material as a result of its low absorption. The responsivity of a state‐of‐the art diamond quadrant transmission detector has been determined, with relative uncertainties below 1% by direct calibration against an electrical substitution radiometer. From these data and the measured transmittance, the thickness of the involved layers as well as the mean electron–hole pair creation energy were determined, the latter with an unprecedented relative uncertainty of 1%. The linearity and X‐ray scattering properties of the device are also described.     

A feasibility study of X‐ray phase‐contrast mammographic tomography at the Imaging and Medical beamline of the Australian Synchrotron

Results are presented of a recent experiment at the Imaging and Medical beamline of the Australian Synchrotron intended to contribute to the implementation of low‐dose high‐sensitivity three‐dimensional mammographic phase‐contrast imaging, initially at synchrotrons and subsequently in hospitals and medical imaging clinics. The effect of such imaging parameters as X‐ray energy, source size, detector resolution, sample‐to‐detector distance, scanning and data processing strategies in the case of propagation‐based phase‐contrast computed tomography (CT) have been tested, quantified, evaluated and optimized using a plastic phantom simulating relevant breast‐tissue characteristics. Analysis of the data collected using a Hamamatsu CMOS Flat Panel Sensor, with a pixel size of 100 µm, revealed the presence of propagation‐based phase contrast and demonstrated significant improvement of the quality of phase‐contrast CT imaging compared with conventional (absorption‐based) CT, at medically acceptable radiation doses.     

Application of an ePix100 detector for coherent scattering using a hard X‐ray free‐electron laser

A prototype ePix100 detector was used in small‐angle scattering geometry to capture speckle patterns from a static sample using the Linac Coherent Light Source (LCLS) hard X‐ray free‐electron laser at 8.34 keV. The average number of detected photons per pixel per pulse was varied over three orders of magnitude from about 23 down to 0.01 to test the detector performance. At high average photon count rates, the speckle contrast was evaluated by analyzing the probability distribution of the pixel counts at a constant scattering vector for single frames. For very low average photon counts of less than 0.2 per pixel, the `droplet algorithm' was first applied to the patterns for correcting the effect of charge sharing, and then the pixel count statistics of multiple frames were analyzed collectively to extract the speckle contrast. Results obtained using both methods agree within the uncertainty intervals, providing strong experimental evidence for the validity of the statistical analysis. More importantly it confirms the suitability of the ePix100 detector for X‐ray coherent scattering experiments, especially at very low count rates with performances surpassing those of previously available LCLS detectors.     

Alignment of low‐dose X‐ray fluorescence tomography images using differential phase contrast

X‐ray fluorescence nanotomography provides unprecedented sensitivity for studies of trace metal distributions in whole biological cells. Dose fractionation, in which one acquires very low dose individual projections and then obtains high statistics reconstructions as signal from a voxel is brought together (Hegerl & Hoppe, 1976), requires accurate alignment of these individual projections so as to correct for rotation stage runout. It is shown here that differential phase contrast at 10.2 keV beam energy offers the potential for accurate cross‐correlation alignment of successive projections, by demonstrating that successive low dose, 3 ms per pixel, images acquired at the same specimen position and rotation angle have a narrower and smoother cross‐correlation function (1.5 pixels FWHM at 300 nm pixel size) than that obtained from zinc fluorescence images (25 pixels FWHM). The differential phase contrast alignment resolution is thus well below the 700 nm × 500 nm beam spot size used in this demonstration, so that dose fractionation should be possible for reduced‐dose, more rapidly acquired, fluorescence nanotomography experiments.     

XDS: a flexible beamline for X‐ray diffraction and spectroscopy at the Brazilian synchrotron

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage‐ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X‐ray spectrum (above ～10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi‐purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X‐ray absorption spectroscopy at energies above 18 keV and high‐resolution diffraction experiments. More recently, new setups and photon‐hungry experiments such as total X‐ray scattering, X‐ray diffraction under high pressures, resonant X‐ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.     

The multi‐purpose hard X‐ray beamline BL10 at the DELTA storage ring

The layout and the characteristics of the hard X‐ray beamline BL10 at the superconducting asymmetric wiggler at the 1.5 GeV Dortmund Electron Accelerator DELTA are described. This beamline is equipped with a Si(111) channel‐cut monochromator and is dedicated to X‐ray studies in the spectral range from ～4 keV to ～16 keV photon energy. There are two different endstations available. While X‐ray absorption studies in different detection modes (transmission, fluorescence, reflectivity) can be performed on a designated table, a six‐axis kappa diffractometer is installed for X‐ray scattering and reflectivity experiments. Different detector set‐ups are integrated into the beamline control software, i.e. gas‐filled ionization chambers, different photodiodes, as well as a Pilatus 2D‐detector are permanently available. The performance of the beamline is illustrated by high‐quality X‐ray absorption spectra from several reference compounds. First applications include temperature‐dependent EXAFS experiments from liquid‐nitrogen temperature in a bath cryostat up to ～660 K by using a dedicated furnace. Besides transmission measurements, fluorescence detection for dilute sample systems as well as surface‐sensitive reflection‐mode experiments are presented.     

Layout and first XRF applications of the BAMline at BESSY II

The first hard x‐ray beamline at BESSY II has been installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a double‐multilayer monochromator and a double‐crystal monochromator. Depending on the application, the two devices are used separately or in‐line. The main applications of the monochromatic radiation with photon energies up to 60 keV are x‐ray fluorescence analysis, micro computed tomography, x‐ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV is available for radiometric applications. Copyright © 2004 John Wiley & Sons, Ltd.     

标定脉冲星导航探测器的荧光X射线光源

为标定X射线脉冲星导航用探测器, 设计了一种荧光X射线源, 该射线源的工作原理是 用X射线管的出射线轰击特定荧光靶材, 从而获得能量一定的荧光X射线, 并以此作为标定探测器的荧光X射线光源. 采用硅漂移半导体探测器在大气环境下测试了按上述原理搭建的荧光X射线光源的能谱分布和光子流量, 从光子流量入手推算了该荧光X射线光源用于真空系统中对探测器进行标定的可行性. 研制出了荧光X射线光源样机, 并在真空系统中对荧光X射线光源样机光子流量做了测试. 在探测距离D_x=300 cm, X射线管管流I_a=200 μA时, 所测得的荧光X射线光源光子流量可达19.57 ph/s@4.51 keV, 25.22 ph/s@5.41 keV, 33.27 ph/s@8.05 keV, 确认了所提方法的可行性, 获得了标定探测器的荧光X射线光源.     

Quantitative studies of pyrocarbon‐coated materials using synchrotron radiation

Phase‐contrast imaging provides enhanced image contrast and is important for non‐destructive evaluation of structural materials. In this paper, experimental results on in‐line phase‐contrast imaging using a synchrotron source (ELETTRA, Italy) for objects required in material science applications are discussed. Experiments have been carried out on two types of samples, pyrocarbon‐coated zirconia and pyrocarbon‐coated alumina microspheres. These have applications in both reactor and industrial fields. The phase‐contrast imaging technique is found to be very useful in visualizing and determining the coating thickness of pyrocarbon on zirconia and alumina microspheres. The experiments were carried out at X‐ray energies of 16, 18 and 20 keV and different object‐to‐detector distances. The results describe the contrast values and signal‐to‐noise ratio for both samples. A comprehensive study was carried out to determine the thickness of the pyrocarbon coating on zirconia and alumina microspheres of diameter 500 µm. The advantages of phase‐contrast images are discussed in terms of contrast and resolution, and a comparison is made with absorption images. The results show considerable improvement in contrast with phase‐contrast imaging as compared with absorption radiography.     

Performance of a four‐element Si drift detector for X‐ray absorption fine‐structure spectroscopy: resolution, maximum count rate,and dead‐time correction with incorporation into the ATHENA data analysis software

The performance of a four‐element Si drift detector for energy‐dispersive fluorescence‐yield X‐ray absorption fine‐structure measurements is reported, operating at the National Institute of Standards and Technology beamline X23A2 at the National Synchrotron Light Source. The detector can acquire X‐ray absorption fine‐structure spectra with a throughput exceeding 4 × 10⁵ counts per second per detector element (>1.6 × 10⁶ total counts per second summed over all four channels). At this count rate the resolution at 6 keV is approximately 220 eV, which adequately resolves the Mn Kα and Kβ fluorescence lines. Accurate dead‐time correction is demonstrated, and it has been incorporated into the ATHENA data analysis program. To maintain counting efficiency and high signal to background, it is suggested that the incoming count rate should not exceed ～70% of the maximum throughput.     

Evaluation of the UFXC32k photon‐counting detector for pump–probe experiments using synchrotron radiation

This paper presents the performance of a single‐photon‐counting hybrid pixel X‐ray detector with synchrotron radiation. The camera was evaluated with respect to time‐resolved experiments, namely pump–probe–probe experiments held at SOLEIL. The UFXC camera shows very good energy resolution of around 1.5 keV and allows the minimum threshold setting to be as low as 3 keV keeping the high‐count‐rate capabilities. Measurements of a synchrotron characteristic filling mode prove the proper separation of an isolated bunch of photons and the usability of the detector in time‐resolved experiments.     

Multimodal hard X‐ray imaging of a mammography phantom at a compact synchrotron light source

The Compact Light Source is a miniature synchrotron producing X‐rays at the interaction point of a counter‐propagating laser pulse and electron bunch through the process of inverse Compton scattering. The small transverse size of the luminous region yields a highly coherent beam with an angular divergence of a few milliradians. The intrinsic monochromaticity and coherence of the produced X‐rays can be exploited in high‐sensitivity differential phase‐contrast imaging with a grating‐based interferometer. Here, the first multimodal X‐ray imaging experiments at the Compact Light Source at a clinically compatible X‐ray energy of 21 keV are reported. Dose‐compatible measurements of a mammography phantom clearly demonstrate an increase in contrast attainable through differential phase and dark‐field imaging over conventional attenuation‐based projections.     

Potential of propagation‐based synchrotron X‐ray phase‐contrast computed tomography for cardiac tissue engineering

Hydrogel‐based cardiac tissue engineering offers great promise for myocardial infarction repair. The ability to visualize engineered systems in vivo in animal models is desired to monitor the performance of cardiac constructs. However, due to the low density and weak X‐ray attenuation of hydrogels, conventional radiography and micro‐computed tomography are unable to visualize the hydrogel cardiac constructs upon their implantation, thus limiting their use in animal systems. This paper presents a study on the optimization of synchrotron X‐ray propagation‐based phase‐contrast imaging computed tomography (PCI‐CT) for three‐dimensional (3D) visualization and assessment of the hydrogel cardiac patches. First, alginate hydrogel was 3D‐printed into cardiac patches, with the pores filled by fibrin. The hydrogel patches were then surgically implanted on rat hearts. A week after surgery, the hearts including patches were excised and embedded in a soft‐tissue‐mimicking gel for imaging by using PCI‐CT at an X‐ray energy of 25 keV. During imaging, the sample‐to‐detector distances, CT‐scan time and the region of interest (ROI) were varied and examined for their effects on both imaging quality and radiation dose. The results showed that phase‐retrieved PCI‐CT images provided edge‐enhancement fringes at a sample‐to‐detector distance of 147 cm that enabled visualization of anatomical and microstructural features of the myocardium and the implanted patch in the tissue‐mimicking gel. For visualization of these features, PCI‐CT offered a significantly higher performance than the dual absorption‐phase and clinical magnetic resonance (3 T) imaging techniques. Furthermore, by reducing the total CT‐scan time and ROI, PCI‐CT was examined for lowering the effective dose, meanwhile without much loss of imaging quality. In effect, the higher soft tissue contrast and low‐dose potential of PCI‐CT has been used along with an acceptable overall animal dose to achieve the high spatial resolution needed for cardiac implant visualization. As a result, PCI‐CT at the identified imaging parameters offers great potential for 3D assessment of microstructural features of hydrogel cardiac patches.     

The EIGER detector for low‐energy electron microscopy and photoemission electron microscopy

EIGER is a single‐photon‐counting hybrid pixel detector developed at the Paul Scherrer Institut, Switzerland. It is designed for applications at synchrotron light sources with photon energies above 5 keV. Features of EIGER include a small pixel size (75 µm × 75 µm), a high frame rate (up to 23 kHz), a small dead‐time between frames (down to 3 µs) and a dynamic range up to 32‐bit. In this article, the use of EIGER as a detector for electrons in low‐energy electron microscopy (LEEM) and photoemission electron microscopy (PEEM) is reported. It is demonstrated that, with only a minimal modification to the sensitive part of the detector, EIGER is able to detect electrons emitted or reflected by the sample and accelerated to 8–20 keV. The imaging capabilities are shown to be superior to the standard microchannel plate detector for these types of applications. This is due to the much higher signal‐to‐noise ratio, better homogeneity and improved dynamic range. In addition, the operation of the EIGER detector is not affected by radiation damage from electrons in the present energy range and guarantees more stable performance over time. To benchmark the detector capabilities, LEEM experiments are performed on selected surfaces and the magnetic and electronic properties of individual iron nanoparticles with sizes ranging from 8 to 22 nm are detected using the PEEM endstation at the Surface/Interface Microscopy (SIM) beamline of the Swiss Light Source.     

Inelastic and elastic scattering differential cross‐sections of 59.5 keV photons for Cu and Zn targets

Differential cross‐sections for incoherent and coherent scattering of 59.54 keV photons were measured for Cu and Zn targets at scattering angles of 40–135° in a reflection geometry setup with a graded shielding arrangement. The ratio of these cross‐sections, which can be determined with higher precision than absolute values, is given. A method was used to determine differential incoherent and coherent scattering cross‐sections of elements. This method is based on simultaneous measurement of fluorescence radiation and scattered radiation, thus avoiding problems with measuring source strength and source‐to‐detector solid angle. The measurements were performed using a point source of Am‐241 radioisotope and an Si(Li) detector. The experimental results, which complement earlier results, were compared with the theories of incoherent scattering function and form factor. Copyright © 2004 John Wiley & Sons, Ltd.     

Improvements of the low‐energy performance of a micro‐focus x‐ray source for XRF analysis with the SEM

X‐ray Fluorescence (XRF) with a scanning electron microscope (SEM) is a valuable completion of the analytical capabilities of SEMs. Small and compact micro‐focus x‐ray sources are mounted to the microscope chamber, and the x‐ray spectra are monitored with conventional EDS systems. Up to now the x‐ray tubes used for the micro‐focus x‐ray sources are equipped with beryllium windows about 100 µm thick. The poly‐capillary x‐ray lenses have their transmission maximum at photon energies around 10 keV. It drops down in both low‐ and high‐energy ranges. Hence, L‐radiation from an Mo or Rh target will be strongly attenuated, and the excitation of fluorescence in the soft x‐ray range becomes very ineffective. A new micro‐focus x‐ray source was developed. It is characterised by a lower self‐absorption in the tube target, thin beryllium windows and an x‐ray optics having a large distance between its foci and the maximum of transmission at about 5 keV. Thus K line fluorescence of light elements becomes effectively excited by the L‐radiation from Mo or Rh tube targets. The detection limit for sodium oxide in glass was found to be below 1 mass%. Copyright © 2009 John Wiley & Sons, Ltd.